Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'ProfD Roland Kramer' _publ_contact_author_address ; Universitat Heidelberg Anorganisch-Chemisches I INF 275 Heidelberg 69120 GERMANY ; _publ_contact_author_email ROLAND.KRAEMER@URZ.UNI-HEIDELBERG.DE _publ_section_title ; Synthesis of a novel dinucleating aminocarboxylate macrocycle and structures of its dinuclear complexes with di- and trivalent transition and lanthanide metal ions ; _publ_author_name 'Roland Kramer' #===END data_jb04 _database_code_depnum_ccdc_archive 'CCDC 247935' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 Fe2 N6 O9, 4(H2 O)' _chemical_formula_sum 'C30 H38 Fe2 N6 O13' _chemical_formula_weight 802.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 13.1670(14) _cell_length_b 20.343(2) _cell_length_c 11.6337(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3116.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8000 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27658 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8092 _reflns_number_gt 6582 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+2.3400P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.60(2) _refine_ls_number_reflns 8092 _refine_ls_number_parameters 464 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.37845(3) 0.39657(2) 0.51402(4) 0.01744(11) Uani 1 1 d . . . Fe2 Fe 0.12614(3) 0.38930(2) 0.62933(4) 0.01909(11) Uani 1 1 d . . . O1 O 0.2513(2) 0.39312(9) 0.5698(3) 0.0208(4) Uani 1 1 d . . . O2 O 0.44319(18) 0.35766(11) 0.6568(3) 0.0230(5) Uani 1 1 d . . . O3 O 0.2540(2) 0.41519(13) 0.2013(3) 0.0330(6) Uani 1 1 d . . . O4 O 0.1650(2) 0.42595(11) 0.7871(3) 0.0266(6) Uani 1 1 d . . . O5 O 0.2594(3) 0.40131(16) 0.9392(3) 0.0574(11) Uani 1 1 d . . . O6 O 0.06235(17) 0.35122(11) 0.4829(3) 0.0247(6) Uani 1 1 d . . . O7 O 0.0115(2) 0.37629(13) 0.3056(3) 0.0325(6) Uani 1 1 d . . . O8 O 0.34175(19) 0.43697(11) 0.3600(2) 0.0224(5) Uani 1 1 d . . . O9 O 0.5000(3) 0.38171(14) 0.8313(3) 0.0422(8) Uani 1 1 d . . . O10 O 0.3620(2) 0.20120(14) 0.1365(4) 0.0485(9) Uani 1 1 d . . . O11 O 0.6071(3) 0.16853(17) 0.1006(4) 0.0469(9) Uani 1 1 d . . . O12 O 0.4116(3) 0.32072(18) 0.0366(4) 0.0543(10) Uani 1 1 d . . . O13 O 0.1597(3) 0.20203(14) 0.0334(4) 0.0450(8) Uani 1 1 d . . . N1 N 0.5311(2) 0.39771(13) 0.4475(3) 0.0201(6) Uani 1 1 d . . . N2 N 0.3842(2) 0.31035(13) 0.3973(3) 0.0197(6) Uani 1 1 d . . . N3 N 0.1275(2) 0.30006(13) 0.7399(3) 0.0218(6) Uani 1 1 d . . . N4 N -0.0252(2) 0.38552(14) 0.7000(3) 0.0240(7) Uani 1 1 d . . . N5 N 0.0484(2) 0.47553(13) 0.5516(3) 0.0207(6) Uani 1 1 d . . . N6 N 0.44723(19) 0.48495(13) 0.5951(3) 0.0184(6) Uani 1 1 d . . . C1 C 0.5965(2) 0.44333(16) 0.4846(3) 0.0213(7) Uani 1 1 d . . . C2 C 0.6948(2) 0.44719(17) 0.4409(4) 0.0234(7) Uani 1 1 d . . . H2 H 0.7400 0.4807 0.4659 0.035(4) Uiso 1 1 calc R . . C3 C 0.7248(3) 0.40121(18) 0.3606(4) 0.0268(8) Uani 1 1 d . . . H3 H 0.7922 0.4021 0.3313 0.035(4) Uiso 1 1 calc R . . C4 C 0.6571(3) 0.35373(19) 0.3225(4) 0.0267(7) Uani 1 1 d . . . H4 H 0.6769 0.3218 0.2673 0.035(4) Uiso 1 1 calc R . . C5 C 0.5589(2) 0.35429(16) 0.3677(3) 0.0206(6) Uani 1 1 d . . . C6 C 0.4771(3) 0.30989(17) 0.3233(4) 0.0254(7) Uani 1 1 d . . . H6A H 0.4583 0.3238 0.2446 0.029(2) Uiso 1 1 calc R . . H6B H 0.5038 0.2645 0.3188 0.029(2) Uiso 1 1 calc R . . C7 C 0.3763(2) 0.24488(16) 0.4521(4) 0.0256(8) Uani 1 1 d . . . H7A H 0.3678 0.2112 0.3914 0.029(2) Uiso 1 1 calc R . . H7B H 0.4404 0.2353 0.4932 0.029(2) Uiso 1 1 calc R . . C8 C 0.2915(3) 0.23981(15) 0.5333(4) 0.0257(8) Uani 1 1 d . . . C9 C 0.2209(3) 0.23692(16) 0.5973(4) 0.0267(8) Uani 1 1 d . . . C10 C 0.1364(3) 0.23647(16) 0.6772(4) 0.0267(8) Uani 1 1 d . . . H10A H 0.1459 0.2004 0.7333 0.029(2) Uiso 1 1 calc R . . H10B H 0.0727 0.2280 0.6345 0.029(2) Uiso 1 1 calc R . . C11 C 0.0368(3) 0.29601(18) 0.8173(4) 0.0320(9) Uani 1 1 d . . . H11A H 0.0103 0.2505 0.8162 0.029(2) Uiso 1 1 calc R . . H11B H 0.0582 0.3060 0.8970 0.029(2) Uiso 1 1 calc R . . C12 C -0.0464(2) 0.34221(16) 0.7835(4) 0.0225(7) Uani 1 1 d . . . C13 C -0.1398(3) 0.34227(18) 0.8389(4) 0.0275(8) Uani 1 1 d . . . H13 H -0.1547 0.3108 0.8968 0.035(4) Uiso 1 1 calc R . . C14 C -0.2109(3) 0.38944(17) 0.8076(4) 0.0285(8) Uani 1 1 d . . . H14 H -0.2752 0.3906 0.8446 0.035(4) Uiso 1 1 calc R . . C15 C -0.1882(3) 0.43468(17) 0.7227(4) 0.0254(7) Uani 1 1 d . . . H15 H -0.2359 0.4675 0.7014 0.035(4) Uiso 1 1 calc R . . C16 C -0.0940(2) 0.43090(16) 0.6694(3) 0.0212(7) Uani 1 1 d . . . C17 C -0.0640(2) 0.47464(18) 0.5718(4) 0.0281(8) Uani 1 1 d . . . H17A H -0.0874 0.5199 0.5882 0.029(2) Uiso 1 1 calc R . . H17B H -0.0985 0.4595 0.5010 0.029(2) Uiso 1 1 calc R . . C18 C 0.0880(2) 0.54109(16) 0.5896(4) 0.0246(7) Uani 1 1 d . . . H18A H 0.0577 0.5760 0.5413 0.029(2) Uiso 1 1 calc R . . H18B H 0.0673 0.5491 0.6702 0.029(2) Uiso 1 1 calc R . . C19 C 0.1993(3) 0.54448(15) 0.5812(4) 0.0224(7) Uani 1 1 d . . . C20 C 0.2888(3) 0.54626(15) 0.5741(3) 0.0207(7) Uani 1 1 d . . . C21 C 0.3991(2) 0.54853(16) 0.5619(4) 0.0210(7) Uani 1 1 d . . . H21A H 0.4266 0.5841 0.6110 0.029(2) Uiso 1 1 calc R . . H21B H 0.4166 0.5588 0.4811 0.029(2) Uiso 1 1 calc R . . C22 C 0.5591(2) 0.49046(18) 0.5734(4) 0.0278(8) Uani 1 1 d . . . H22A H 0.5748 0.5358 0.5481 0.029(2) Uiso 1 1 calc R . . H22B H 0.5960 0.4824 0.6462 0.029(2) Uiso 1 1 calc R . . C23 C 0.2935(3) 0.32557(16) 0.3251(3) 0.0223(7) Uani 1 1 d . . . H23A H 0.2307 0.3162 0.3690 0.029(2) Uiso 1 1 calc R . . H23B H 0.2937 0.2975 0.2556 0.029(2) Uiso 1 1 calc R . . C24 C 0.2957(3) 0.39785(15) 0.2901(4) 0.0219(7) Uani 1 1 d . . . C25 C 0.2186(3) 0.31503(16) 0.8098(4) 0.0251(7) Uani 1 1 d . . . H25A H 0.2806 0.3080 0.7632 0.029(2) Uiso 1 1 calc R . . H25B H 0.2215 0.2852 0.8770 0.029(2) Uiso 1 1 calc R . . C26 C 0.2146(3) 0.38596(18) 0.8507(4) 0.0303(9) Uani 1 1 d . . . C27 C 0.0676(3) 0.46390(17) 0.4274(4) 0.0242(7) Uani 1 1 d . . . H27A H 0.1392 0.4740 0.4086 0.029(2) Uiso 1 1 calc R . . H27B H 0.0233 0.4926 0.3804 0.029(2) Uiso 1 1 calc R . . C28 C 0.0447(3) 0.39126(16) 0.4017(4) 0.0230(8) Uani 1 1 d . . . C29 C 0.4311(3) 0.46891(15) 0.7179(4) 0.0215(7) Uani 1 1 d . . . H29A H 0.3588 0.4753 0.7382 0.029(2) Uiso 1 1 calc R . . H29B H 0.4725 0.4985 0.7666 0.029(2) Uiso 1 1 calc R . . C30 C 0.4616(3) 0.39774(15) 0.7397(4) 0.0234(8) Uani 1 1 d . . . H101 H 0.3809 0.2379 0.1015 0.080(7) Uiso 1 1 d . . . H102 H 0.4219 0.1845 0.1766 0.080(7) Uiso 1 1 d . . . H111 H 0.6772 0.1495 0.1233 0.080(7) Uiso 1 1 d . . . H112 H 0.5787 0.1653 0.1589 0.080(7) Uiso 1 1 d . . . H121 H 0.4398 0.3275 -0.0206 0.080(7) Uiso 1 1 d . . . H122 H 0.3441 0.3379 0.0245 0.080(7) Uiso 1 1 d . . . H131 H 0.1269 0.2389 0.0467 0.080(7) Uiso 1 1 d . . . H132 H 0.2239 0.1986 0.0555 0.080(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0161(2) 0.01692(18) 0.0193(3) -0.00356(18) -0.0018(2) 0.00058(14) Fe2 0.0157(2) 0.01786(19) 0.0237(3) 0.00556(19) 0.0009(2) -0.00024(14) O1 0.0179(8) 0.0188(8) 0.0255(11) 0.0007(10) 0.0003(7) 0.0006(9) O2 0.0221(11) 0.0193(10) 0.0275(15) -0.0042(9) -0.0058(10) 0.0037(8) O3 0.0471(16) 0.0266(13) 0.0253(16) 0.0015(11) -0.0100(13) 0.0023(11) O4 0.0313(12) 0.0222(11) 0.0262(15) 0.0021(11) 0.0032(11) -0.0020(9) O5 0.106(3) 0.0330(16) 0.033(2) 0.0008(14) -0.030(2) -0.0067(17) O6 0.0225(11) 0.0183(10) 0.0333(17) 0.0027(10) -0.0052(11) -0.0040(8) O7 0.0385(15) 0.0307(13) 0.0283(16) -0.0014(13) -0.0071(13) -0.0026(11) O8 0.0283(12) 0.0183(10) 0.0206(13) -0.0022(9) -0.0011(10) 0.0004(9) O9 0.061(2) 0.0319(14) 0.034(2) 0.0002(13) -0.0203(16) 0.0070(13) O10 0.0443(16) 0.0362(14) 0.065(3) -0.0158(18) -0.0035(17) 0.0002(12) O11 0.0506(17) 0.0481(17) 0.042(2) 0.0131(16) -0.0066(16) -0.0040(14) O12 0.057(2) 0.065(2) 0.040(2) 0.0110(18) -0.0031(17) -0.0175(17) O13 0.0504(17) 0.0328(14) 0.052(2) 0.0055(15) -0.0048(16) -0.0021(13) N1 0.0189(12) 0.0231(13) 0.0184(15) -0.0034(11) -0.0002(11) 0.0030(10) N2 0.0204(12) 0.0176(11) 0.0210(15) -0.0036(11) -0.0018(11) 0.0017(9) N3 0.0186(12) 0.0208(12) 0.0258(17) 0.0067(11) -0.0001(11) -0.0030(9) N4 0.0189(13) 0.0222(13) 0.031(2) 0.0069(12) -0.0017(13) -0.0028(10) N5 0.0150(12) 0.0187(12) 0.0285(18) 0.0047(11) 0.0006(11) -0.0006(9) N6 0.0152(11) 0.0176(11) 0.0224(16) -0.0038(10) 0.0011(11) -0.0012(9) C1 0.0159(13) 0.0234(14) 0.0247(18) 0.0016(13) -0.0027(13) 0.0010(11) C2 0.0154(14) 0.0309(16) 0.0238(18) 0.0061(14) 0.0011(13) -0.0007(12) C3 0.0203(15) 0.0353(18) 0.0247(19) 0.0071(15) 0.0052(14) 0.0039(13) C4 0.0252(15) 0.0322(16) 0.0226(18) -0.0007(14) 0.0023(14) 0.0074(14) C5 0.0183(14) 0.0252(15) 0.0184(17) 0.0004(13) -0.0018(12) 0.0050(11) C6 0.0236(15) 0.0284(16) 0.0241(19) -0.0105(14) 0.0028(14) 0.0033(12) C7 0.0278(17) 0.0168(14) 0.032(2) -0.0007(13) -0.0038(14) 0.0060(12) C8 0.0334(17) 0.0146(13) 0.029(2) 0.0005(13) -0.0056(16) 0.0000(12) C9 0.0353(18) 0.0174(13) 0.027(2) 0.0011(13) -0.0069(14) -0.0018(12) C10 0.0330(18) 0.0166(14) 0.031(2) 0.0025(13) -0.0038(15) -0.0055(12) C11 0.0295(17) 0.0308(17) 0.036(2) 0.0150(17) 0.0064(16) 0.0005(14) C12 0.0242(15) 0.0228(14) 0.0205(18) 0.0013(13) 0.0009(13) -0.0047(11) C13 0.0308(17) 0.0302(17) 0.0215(19) -0.0039(14) 0.0054(14) -0.0104(13) C14 0.0231(16) 0.0354(18) 0.027(2) -0.0074(15) 0.0067(14) -0.0077(13) C15 0.0195(15) 0.0291(16) 0.0276(19) -0.0079(15) 0.0021(14) -0.0011(12) C16 0.0163(14) 0.0234(15) 0.0241(18) 0.0004(13) 0.0010(12) -0.0033(11) C17 0.0146(13) 0.0321(17) 0.038(2) 0.0079(16) -0.0003(14) 0.0036(12) C18 0.0231(15) 0.0190(14) 0.032(2) 0.0002(13) -0.0007(14) 0.0023(11) C19 0.0290(17) 0.0144(13) 0.0238(19) 0.0008(12) -0.0010(14) 0.0003(12) C20 0.0238(14) 0.0149(13) 0.0234(19) 0.0006(12) -0.0022(14) 0.0005(11) C21 0.0184(13) 0.0182(13) 0.0265(19) 0.0025(13) 0.0011(13) -0.0007(11) C22 0.0142(13) 0.0338(18) 0.035(2) -0.0131(16) -0.0004(14) -0.0036(12) C23 0.0233(15) 0.0221(14) 0.0216(18) -0.0051(13) -0.0064(13) 0.0015(12) C24 0.0241(16) 0.0203(14) 0.0212(19) -0.0015(13) 0.0004(14) 0.0024(11) C25 0.0300(16) 0.0212(14) 0.0242(19) 0.0030(14) -0.0054(14) -0.0027(12) C26 0.043(2) 0.0249(17) 0.023(2) 0.0021(14) -0.0005(17) -0.0074(15) C27 0.0242(16) 0.0229(15) 0.026(2) 0.0055(14) -0.0021(15) -0.0019(12) C28 0.0191(15) 0.0208(15) 0.029(2) 0.0031(13) 0.0018(15) 0.0003(11) C29 0.0258(16) 0.0193(14) 0.0195(18) -0.0035(13) -0.0028(14) 0.0021(11) C30 0.0263(16) 0.0190(14) 0.025(2) -0.0002(13) -0.0065(15) 0.0033(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.797(3) . ? Fe1 O2 2.028(3) . ? Fe1 O8 2.030(3) . ? Fe1 N1 2.154(3) . ? Fe1 N2 2.219(3) . ? Fe1 N6 2.223(3) . ? Fe2 O1 1.789(3) . ? Fe2 O4 2.046(3) . ? Fe2 O6 2.051(3) . ? Fe2 N4 2.157(3) . ? Fe2 N5 2.223(3) . ? Fe2 N3 2.225(3) . ? O2 C30 1.286(5) . ? O3 C24 1.222(5) . ? O4 C26 1.279(5) . ? O5 C26 1.227(6) . ? O6 C28 1.269(5) . ? O7 C28 1.238(6) . ? O8 C24 1.289(4) . ? O9 C30 1.225(5) . ? O10 H101 0.88 . ? O10 H102 0.98 . ? O11 H111 1.04 . ? O11 H112 0.78 . ? O12 H121 0.77 . ? O12 H122 0.97 . ? O13 H131 0.88 . ? O13 H132 0.89 . ? N1 C5 1.333(5) . ? N1 C1 1.337(4) . ? N2 C7 1.480(4) . ? N2 C23 1.493(4) . ? N2 C6 1.496(5) . ? N3 C25 1.482(5) . ? N3 C10 1.490(5) . ? N3 C11 1.497(5) . ? N4 C12 1.341(5) . ? N4 C16 1.341(4) . ? N5 C27 1.485(5) . ? N5 C18 1.499(4) . ? N5 C17 1.499(4) . ? N6 C29 1.481(5) . ? N6 C21 1.491(4) . ? N6 C22 1.499(4) . ? C1 C2 1.392(5) . ? C1 C22 1.493(5) . ? C2 C3 1.380(6) . ? C2 H2 0.9500 . ? C3 C4 1.388(5) . ? C3 H3 0.9500 . ? C4 C5 1.395(5) . ? C4 H4 0.9500 . ? C5 C6 1.498(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.467(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.192(5) . ? C9 C10 1.450(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.496(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.388(5) . ? C13 C14 1.389(6) . ? C13 H13 0.9500 . ? C14 C15 1.383(6) . ? C14 H14 0.9500 . ? C15 C16 1.390(5) . ? C15 H15 0.9500 . ? C16 C17 1.495(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.470(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.182(4) . ? C20 C21 1.460(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.526(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C25 C26 1.520(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 C28 1.538(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C29 C30 1.523(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 94.61(14) . . ? O1 Fe1 O8 96.49(13) . . ? O2 Fe1 O8 168.89(11) . . ? O1 Fe1 N1 178.37(10) . . ? O2 Fe1 N1 84.62(12) . . ? O8 Fe1 N1 84.30(12) . . ? O1 Fe1 N2 102.82(11) . . ? O2 Fe1 N2 100.26(10) . . ? O8 Fe1 N2 77.77(11) . . ? N1 Fe1 N2 75.94(11) . . ? O1 Fe1 N6 104.93(11) . . ? O2 Fe1 N6 78.28(10) . . ? O8 Fe1 N6 98.29(10) . . ? N1 Fe1 N6 76.32(10) . . ? N2 Fe1 N6 152.24(10) . . ? O1 Fe2 O4 95.80(14) . . ? O1 Fe2 O6 94.14(14) . . ? O4 Fe2 O6 170.05(11) . . ? O1 Fe2 N4 179.41(14) . . ? O4 Fe2 N4 84.39(13) . . ? O6 Fe2 N4 85.67(12) . . ? O1 Fe2 N5 103.42(11) . . ? O4 Fe2 N5 101.11(11) . . ? O6 Fe2 N5 76.79(11) . . ? N4 Fe2 N5 75.99(11) . . ? O1 Fe2 N3 104.60(11) . . ? O4 Fe2 N3 77.09(11) . . ? O6 Fe2 N3 100.10(11) . . ? N4 Fe2 N3 75.99(11) . . ? N5 Fe2 N3 151.96(10) . . ? Fe2 O1 Fe1 178.4(2) . . ? C30 O2 Fe1 116.5(2) . . ? C26 O4 Fe2 114.5(2) . . ? C28 O6 Fe2 116.8(2) . . ? C24 O8 Fe1 114.8(2) . . ? H101 O10 H102 107 . . ? H111 O11 H112 100 . . ? H121 O12 H122 105 . . ? H131 O13 H132 119 . . ? C5 N1 C1 120.5(3) . . ? C5 N1 Fe1 120.0(2) . . ? C1 N1 Fe1 119.5(2) . . ? C7 N2 C23 111.9(3) . . ? C7 N2 C6 107.4(3) . . ? C23 N2 C6 109.3(3) . . ? C7 N2 Fe1 116.5(3) . . ? C23 N2 Fe1 98.81(18) . . ? C6 N2 Fe1 112.64(19) . . ? C25 N3 C10 112.5(3) . . ? C25 N3 C11 109.1(3) . . ? C10 N3 C11 108.0(3) . . ? C25 N3 Fe2 98.98(19) . . ? C10 N3 Fe2 115.2(3) . . ? C11 N3 Fe2 112.7(2) . . ? C12 N4 C16 120.3(3) . . ? C12 N4 Fe2 119.4(2) . . ? C16 N4 Fe2 119.9(2) . . ? C27 N5 C18 111.7(3) . . ? C27 N5 C17 108.6(3) . . ? C18 N5 C17 107.9(3) . . ? C27 N5 Fe2 101.1(2) . . ? C18 N5 Fe2 114.9(2) . . ? C17 N5 Fe2 112.4(2) . . ? C29 N6 C21 112.4(3) . . ? C29 N6 C22 108.7(3) . . ? C21 N6 C22 108.0(3) . . ? C29 N6 Fe1 99.96(19) . . ? C21 N6 Fe1 114.7(2) . . ? C22 N6 Fe1 112.9(2) . . ? N1 C1 C2 121.3(3) . . ? N1 C1 C22 117.2(3) . . ? C2 C1 C22 121.5(3) . . ? C3 C2 C1 118.4(3) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 120.2(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 118.0(4) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? N1 C5 C4 121.5(3) . . ? N1 C5 C6 116.3(3) . . ? C4 C5 C6 122.1(3) . . ? N2 C6 C5 112.7(3) . . ? N2 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N2 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C8 C7 N2 113.2(3) . . ? C8 C7 H7A 108.9 . . ? N2 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? N2 C7 H7B 108.9 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C7 178.1(4) . . ? C8 C9 C10 177.3(4) . . ? C9 C10 N3 111.6(3) . . ? C9 C10 H10A 109.3 . . ? N3 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? N3 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C12 C11 N3 113.0(3) . . ? C12 C11 H11A 109.0 . . ? N3 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? N3 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N4 C12 C13 121.3(3) . . ? N4 C12 C11 116.8(3) . . ? C13 C12 C11 121.8(3) . . ? C12 C13 C14 118.5(4) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 120.1(4) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 118.4(3) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? N4 C16 C15 121.5(3) . . ? N4 C16 C17 115.7(3) . . ? C15 C16 C17 122.8(3) . . ? C16 C17 N5 112.8(3) . . ? C16 C17 H17A 109.0 . . ? N5 C17 H17A 109.0 . . ? C16 C17 H17B 109.0 . . ? N5 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C19 C18 N5 111.6(3) . . ? C19 C18 H18A 109.3 . . ? N5 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? N5 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C20 C19 C18 179.1(4) . . ? C19 C20 C21 178.5(4) . . ? C20 C21 N6 111.7(3) . . ? C20 C21 H21A 109.3 . . ? N6 C21 H21A 109.3 . . ? C20 C21 H21B 109.3 . . ? N6 C21 H21B 109.3 . . ? H21A C21 H21B 107.9 . . ? C1 C22 N6 113.1(3) . . ? C1 C22 H22A 109.0 . . ? N6 C22 H22A 109.0 . . ? C1 C22 H22B 109.0 . . ? N6 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? N2 C23 C24 109.6(3) . . ? N2 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? N2 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? O3 C24 O8 124.5(3) . . ? O3 C24 C23 119.7(3) . . ? O8 C24 C23 115.8(3) . . ? N3 C25 C26 109.8(3) . . ? N3 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? N3 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? O5 C26 O4 124.7(4) . . ? O5 C26 C25 119.1(4) . . ? O4 C26 C25 116.2(4) . . ? N5 C27 C28 108.0(3) . . ? N5 C27 H27A 110.1 . . ? C28 C27 H27A 110.1 . . ? N5 C27 H27B 110.1 . . ? C28 C27 H27B 110.1 . . ? H27A C27 H27B 108.4 . . ? O7 C28 O6 125.4(3) . . ? O7 C28 C27 118.8(3) . . ? O6 C28 C27 115.8(4) . . ? N6 C29 C30 109.4(3) . . ? N6 C29 H29A 109.8 . . ? C30 C29 H29A 109.8 . . ? N6 C29 H29B 109.8 . . ? C30 C29 H29B 109.8 . . ? H29A C29 H29B 108.2 . . ? O9 C30 O2 124.2(3) . . ? O9 C30 C29 120.4(3) . . ? O2 C30 C29 115.4(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.639 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.089 data_jb05 _database_code_depnum_ccdc_archive 'CCDC 247936' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H66 N6 O8' _chemical_formula_sum 'C46 H66 N6 O8' _chemical_formula_weight 831.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.2177(7) _cell_length_b 11.8051(12) _cell_length_c 16.2832(17) _cell_angle_alpha 93.933(2) _cell_angle_beta 97.753(2) _cell_angle_gamma 100.204(2) _cell_volume 1160.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8627 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19422 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 30.50 _reflns_number_total 7041 _reflns_number_gt 5002 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.3290P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7041 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1283 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.54962(17) 0.70794(8) 0.54419(6) 0.0242(2) Uani 1 1 d . . . N2 N 0.79668(17) 0.80124(9) 0.38728(6) 0.0235(2) Uani 1 1 d . . . N3 N 0.89104(17) 0.36955(9) 0.33112(6) 0.0246(2) Uani 1 1 d . . . C1 C 0.3905(2) 0.72387(10) 0.58940(7) 0.0240(2) Uani 1 1 d . . . C2 C 0.3664(2) 0.83278(11) 0.62138(8) 0.0280(3) Uani 1 1 d . . . C3 C 0.5124(3) 0.92899(11) 0.60502(9) 0.0341(3) Uani 1 1 d . . . C4 C 0.6748(3) 0.91322(11) 0.55721(8) 0.0325(3) Uani 1 1 d . . . C5 C 0.6886(2) 0.80170(10) 0.52793(7) 0.0245(2) Uani 1 1 d . . . C6 C 0.8588(2) 0.77936(11) 0.47456(8) 0.0267(2) Uani 1 1 d . . . C7 C 0.9763(2) 0.78742(11) 0.33945(8) 0.0272(3) Uani 1 1 d . . . C8 C 1.0304(2) 0.67037(11) 0.33709(8) 0.0261(2) Uani 1 1 d . . . C9 C 1.0677(2) 0.57448(11) 0.33856(8) 0.0262(2) Uani 1 1 d . . . C10 C 1.0989(2) 0.45320(11) 0.33901(8) 0.0271(3) Uani 1 1 d . . . C11 C 0.7672(2) 0.38544(10) 0.39947(8) 0.0257(2) Uani 1 1 d . . . C12 C 0.5928(2) 0.72150(11) 0.35088(7) 0.0253(2) Uani 1 1 d . . . C13 C 0.5100(2) 0.74722(11) 0.26366(8) 0.0273(3) Uani 1 1 d . . . C14 C 0.3719(2) 0.65053(12) 0.12301(7) 0.0283(3) Uani 1 1 d . . . C15 C 0.3400(4) 0.52357(15) 0.09117(11) 0.0499(4) Uani 1 1 d . . . C16 C 0.1507(3) 0.6886(2) 0.11549(10) 0.0467(4) Uani 1 1 d . . . C17 C 0.5382(3) 0.72336(16) 0.07936(9) 0.0411(4) Uani 1 1 d . . . C18 C 0.7563(2) 0.36783(11) 0.25057(8) 0.0280(3) Uani 1 1 d . . . C19 C 0.8319(2) 0.30210(11) 0.17989(8) 0.0286(3) Uani 1 1 d . . . C20 C 0.9739(3) 0.12578(13) 0.14656(9) 0.0404(3) Uani 1 1 d . . . C21 C 1.1690(3) 0.18555(17) 0.10909(14) 0.0598(5) Uani 1 1 d . . . H21A H 1.1203 0.2403 0.0714 0.096(3) Uiso 1 1 calc R . . H21B H 1.2298 0.1277 0.0780 0.096(3) Uiso 1 1 calc R . . H21C H 1.2830 0.2273 0.1537 0.096(3) Uiso 1 1 calc R . . C22 C 0.7809(3) 0.07330(16) 0.08012(13) 0.0623(5) Uani 1 1 d . . . H22A H 0.6515 0.0450 0.1065 0.096(3) Uiso 1 1 calc R . . H22B H 0.8191 0.0088 0.0476 0.096(3) Uiso 1 1 calc R . . H22C H 0.7470 0.1321 0.0433 0.096(3) Uiso 1 1 calc R . . C23 C 1.0323(6) 0.0363(2) 0.20253(14) 0.0892(9) Uani 1 1 d . . . H23A H 1.1581 0.0713 0.2449 0.096(3) Uiso 1 1 calc R . . H23B H 1.0717 -0.0274 0.1695 0.096(3) Uiso 1 1 calc R . . H23C H 0.9052 0.0066 0.2297 0.096(3) Uiso 1 1 calc R . . O1 O 0.4869(2) 0.84173(9) 0.24479(6) 0.0475(3) Uani 1 1 d . . . O2 O 0.46375(15) 0.65051(7) 0.21197(5) 0.02618(19) Uani 1 1 d . . . O3 O 0.8170(2) 0.33062(10) 0.11027(6) 0.0454(3) Uani 1 1 d . . . O4 O 0.9051(2) 0.20936(9) 0.20476(6) 0.0405(3) Uani 1 1 d . . . H2 H 0.251(3) 0.8405(13) 0.6538(9) 0.029(4) Uiso 1 1 d . . . H3 H 0.498(3) 1.0044(16) 0.6268(11) 0.045(5) Uiso 1 1 d . . . H4 H 0.786(3) 0.9780(16) 0.5424(11) 0.047(5) Uiso 1 1 d . . . H6A H 0.878(3) 0.6946(14) 0.4785(10) 0.036(4) Uiso 1 1 d . . . H6B H 1.004(3) 0.8325(14) 0.4959(10) 0.038(4) Uiso 1 1 d . . . H7A H 0.936(2) 0.8074(13) 0.2822(10) 0.030(4) Uiso 1 1 d . . . H7B H 1.109(3) 0.8404(14) 0.3651(10) 0.037(4) Uiso 1 1 d . . . H10A H 1.177(3) 0.4328(14) 0.2928(10) 0.034(4) Uiso 1 1 d . . . H10B H 1.192(3) 0.4421(13) 0.3902(10) 0.035(4) Uiso 1 1 d . . . H11A H 0.878(2) 0.4064(13) 0.4518(9) 0.028(4) Uiso 1 1 d . . . H11B H 0.678(3) 0.4491(14) 0.3934(10) 0.036(4) Uiso 1 1 d . . . H12A H 0.482(2) 0.7317(12) 0.3851(9) 0.026(4) Uiso 1 1 d . . . H12B H 0.609(2) 0.6397(14) 0.3508(9) 0.030(4) Uiso 1 1 d . . . H15A H 0.281(3) 0.5127(16) 0.0310(12) 0.053(5) Uiso 1 1 d . . . H15B H 0.496(4) 0.500(2) 0.0975(14) 0.076(7) Uiso 1 1 d . . . H15C H 0.231(4) 0.479(2) 0.1228(14) 0.076(7) Uiso 1 1 d . . . H16A H 0.083(3) 0.6768(16) 0.0552(12) 0.052(5) Uiso 1 1 d . . . H16B H 0.178(3) 0.7716(18) 0.1322(12) 0.053(5) Uiso 1 1 d . . . H16C H 0.053(4) 0.644(2) 0.1502(15) 0.077(7) Uiso 1 1 d . . . H17A H 0.483(3) 0.7124(14) 0.0200(11) 0.041(4) Uiso 1 1 d . . . H17B H 0.557(3) 0.8053(18) 0.1000(12) 0.054(5) Uiso 1 1 d . . . H17C H 0.680(3) 0.6976(17) 0.0890(12) 0.057(5) Uiso 1 1 d . . . H18A H 0.604(3) 0.3268(13) 0.2543(9) 0.032(4) Uiso 1 1 d . . . H18B H 0.738(3) 0.4442(15) 0.2342(11) 0.043(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0297(5) 0.0209(5) 0.0215(5) 0.0020(4) 0.0028(4) 0.0044(4) N2 0.0246(5) 0.0226(5) 0.0232(5) 0.0010(4) 0.0054(4) 0.0032(4) N3 0.0289(5) 0.0214(5) 0.0234(5) 0.0014(4) 0.0046(4) 0.0040(4) C1 0.0309(6) 0.0198(5) 0.0207(5) 0.0020(4) 0.0027(4) 0.0044(4) C2 0.0374(7) 0.0221(6) 0.0257(6) 0.0012(4) 0.0085(5) 0.0062(5) C3 0.0509(8) 0.0186(6) 0.0333(7) -0.0012(5) 0.0120(6) 0.0046(5) C4 0.0442(8) 0.0198(6) 0.0319(6) 0.0000(5) 0.0105(6) -0.0011(5) C5 0.0297(6) 0.0230(6) 0.0194(5) 0.0015(4) 0.0014(4) 0.0032(5) C6 0.0261(6) 0.0279(6) 0.0248(6) 0.0018(5) 0.0017(5) 0.0036(5) C7 0.0291(6) 0.0206(6) 0.0330(6) 0.0031(5) 0.0116(5) 0.0018(5) C8 0.0233(6) 0.0256(6) 0.0300(6) 0.0016(5) 0.0097(5) 0.0019(5) C9 0.0237(6) 0.0256(6) 0.0293(6) 0.0021(5) 0.0080(5) 0.0018(5) C10 0.0258(6) 0.0243(6) 0.0323(6) 0.0022(5) 0.0067(5) 0.0062(5) C11 0.0324(6) 0.0187(5) 0.0264(6) 0.0003(4) 0.0071(5) 0.0044(5) C12 0.0257(6) 0.0259(6) 0.0231(5) 0.0015(4) 0.0035(4) 0.0026(5) C13 0.0311(6) 0.0264(6) 0.0246(6) -0.0006(5) 0.0027(5) 0.0083(5) C14 0.0289(6) 0.0350(7) 0.0203(5) -0.0014(5) 0.0032(4) 0.0058(5) C15 0.0713(12) 0.0399(9) 0.0318(8) -0.0091(6) 0.0017(8) 0.0021(8) C16 0.0330(8) 0.0770(13) 0.0320(7) 0.0018(8) 0.0019(6) 0.0193(8) C17 0.0379(8) 0.0552(10) 0.0291(7) 0.0094(7) 0.0071(6) 0.0018(7) C18 0.0327(7) 0.0254(6) 0.0258(6) 0.0027(5) 0.0030(5) 0.0060(5) C19 0.0343(7) 0.0239(6) 0.0257(6) 0.0018(5) 0.0034(5) 0.0015(5) C20 0.0605(10) 0.0309(7) 0.0327(7) -0.0031(5) 0.0112(7) 0.0155(7) C21 0.0487(10) 0.0553(11) 0.0745(13) -0.0160(9) 0.0195(9) 0.0079(8) C22 0.0646(12) 0.0416(10) 0.0722(13) -0.0239(9) 0.0061(10) 0.0009(8) C23 0.170(3) 0.0637(14) 0.0578(12) 0.0131(10) 0.0273(15) 0.0772(17) O1 0.0799(8) 0.0290(5) 0.0328(5) 0.0001(4) -0.0068(5) 0.0204(5) O2 0.0308(5) 0.0261(4) 0.0216(4) -0.0004(3) 0.0038(3) 0.0066(3) O3 0.0697(8) 0.0444(6) 0.0257(5) 0.0070(4) 0.0083(5) 0.0186(6) O4 0.0704(7) 0.0308(5) 0.0265(5) 0.0041(4) 0.0133(5) 0.0214(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.3415(16) . ? N1 C5 1.3435(16) . ? N2 C12 1.4635(16) . ? N2 C7 1.4702(16) . ? N2 C6 1.4742(15) . ? N3 C18 1.4547(16) . ? N3 C11 1.4564(16) . ? N3 C10 1.4655(16) . ? C1 C2 1.3942(17) . ? C1 C11 1.5135(17) 2_666 ? C2 C3 1.3878(19) . ? C2 H2 0.958(16) . ? C3 C4 1.386(2) . ? C3 H3 0.960(18) . ? C4 C5 1.3903(18) . ? C4 H4 1.000(19) . ? C5 C6 1.5031(18) . ? C6 H6A 1.035(16) . ? C6 H6B 1.005(17) . ? C7 C8 1.4783(18) . ? C7 H7A 0.988(16) . ? C7 H7B 0.967(17) . ? C8 C9 1.1963(17) . ? C9 C10 1.4789(17) . ? C10 H10A 0.989(16) . ? C10 H10B 0.980(16) . ? C11 C1 1.5135(17) 2_666 ? C11 H11A 1.008(15) . ? C11 H11B 1.014(16) . ? C12 C13 1.5139(17) . ? C12 H12A 0.963(15) . ? C12 H12B 0.988(15) . ? C13 O1 1.2049(16) . ? C13 O2 1.3346(15) . ? C14 O2 1.4838(14) . ? C14 C17 1.510(2) . ? C14 C16 1.513(2) . ? C14 C15 1.521(2) . ? C15 H15A 0.99(2) . ? C15 H15B 1.05(2) . ? C15 H15C 1.00(2) . ? C16 H16A 1.005(19) . ? C16 H16B 0.98(2) . ? C16 H16C 1.00(2) . ? C17 H17A 0.973(17) . ? C17 H17B 0.98(2) . ? C17 H17C 0.98(2) . ? C18 C19 1.5167(18) . ? C18 H18A 0.997(16) . ? C18 H18B 0.979(17) . ? C19 O3 1.2008(16) . ? C19 O4 1.3257(16) . ? C20 O4 1.4781(17) . ? C20 C23 1.502(2) . ? C20 C22 1.513(3) . ? C20 C21 1.516(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C5 118.15(10) . . ? C12 N2 C7 110.44(10) . . ? C12 N2 C6 109.69(10) . . ? C7 N2 C6 110.05(10) . . ? C18 N3 C11 111.76(10) . . ? C18 N3 C10 111.69(10) . . ? C11 N3 C10 112.98(10) . . ? N1 C1 C2 122.91(11) . . ? N1 C1 C11 114.79(10) . 2_666 ? C2 C1 C11 122.26(11) . 2_666 ? C3 C2 C1 118.50(12) . . ? C3 C2 H2 121.1(9) . . ? C1 C2 H2 120.4(9) . . ? C4 C3 C2 118.85(12) . . ? C4 C3 H3 121.8(11) . . ? C2 C3 H3 119.3(11) . . ? C3 C4 C5 119.16(12) . . ? C3 C4 H4 123.7(10) . . ? C5 C4 H4 117.1(10) . . ? N1 C5 C4 122.41(12) . . ? N1 C5 C6 116.01(11) . . ? C4 C5 C6 121.56(12) . . ? N2 C6 C5 112.27(10) . . ? N2 C6 H6A 110.9(9) . . ? C5 C6 H6A 107.9(9) . . ? N2 C6 H6B 107.0(9) . . ? C5 C6 H6B 109.7(9) . . ? H6A C6 H6B 109.1(13) . . ? N2 C7 C8 113.92(10) . . ? N2 C7 H7A 108.8(9) . . ? C8 C7 H7A 109.9(9) . . ? N2 C7 H7B 108.7(10) . . ? C8 C7 H7B 106.7(10) . . ? H7A C7 H7B 108.7(13) . . ? C9 C8 C7 176.50(13) . . ? C8 C9 C10 176.43(13) . . ? N3 C10 C9 113.41(10) . . ? N3 C10 H10A 107.7(9) . . ? C9 C10 H10A 110.5(9) . . ? N3 C10 H10B 108.1(9) . . ? C9 C10 H10B 110.9(9) . . ? H10A C10 H10B 106.0(13) . . ? N3 C11 C1 112.22(10) . 2_666 ? N3 C11 H11A 107.0(9) . . ? C1 C11 H11A 108.1(9) 2_666 . ? N3 C11 H11B 113.9(9) . . ? C1 C11 H11B 107.3(9) 2_666 . ? H11A C11 H11B 108.2(12) . . ? N2 C12 C13 111.94(10) . . ? N2 C12 H12A 107.6(9) . . ? C13 C12 H12A 107.7(9) . . ? N2 C12 H12B 112.5(9) . . ? C13 C12 H12B 110.0(9) . . ? H12A C12 H12B 106.9(12) . . ? O1 C13 O2 125.52(12) . . ? O1 C13 C12 124.18(11) . . ? O2 C13 C12 110.29(10) . . ? O2 C14 C17 109.80(11) . . ? O2 C14 C16 110.19(11) . . ? C17 C14 C16 113.38(14) . . ? O2 C14 C15 102.39(11) . . ? C17 C14 C15 110.63(14) . . ? C16 C14 C15 109.90(15) . . ? C14 C15 H15A 110.0(11) . . ? C14 C15 H15B 107.6(13) . . ? H15A C15 H15B 106.9(17) . . ? C14 C15 H15C 107.2(13) . . ? H15A C15 H15C 109.7(17) . . ? H15B C15 H15C 115.4(18) . . ? C14 C16 H16A 108.2(11) . . ? C14 C16 H16B 107.8(12) . . ? H16A C16 H16B 107.3(16) . . ? C14 C16 H16C 110.4(14) . . ? H16A C16 H16C 111.0(17) . . ? H16B C16 H16C 112.0(17) . . ? C14 C17 H17A 107.9(10) . . ? C14 C17 H17B 110.1(11) . . ? H17A C17 H17B 110.2(15) . . ? C14 C17 H17C 109.6(12) . . ? H17A C17 H17C 108.9(15) . . ? H17B C17 H17C 110.1(16) . . ? N3 C18 C19 114.07(11) . . ? N3 C18 H18A 107.9(9) . . ? C19 C18 H18A 105.9(9) . . ? N3 C18 H18B 114.5(10) . . ? C19 C18 H18B 108.8(10) . . ? H18A C18 H18B 104.9(13) . . ? O3 C19 O4 125.96(13) . . ? O3 C19 C18 122.66(12) . . ? O4 C19 C18 111.33(11) . . ? O4 C20 C23 102.07(13) . . ? O4 C20 C22 109.76(14) . . ? C23 C20 C22 110.38(18) . . ? O4 C20 C21 109.67(13) . . ? C23 C20 C21 112.92(18) . . ? C22 C20 C21 111.62(15) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C13 O2 C14 121.45(10) . . ? C19 O4 C20 122.22(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.369 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.044 #===END data_jb10 _database_code_depnum_ccdc_archive 'CCDC 247937' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 N6 O8 Zn2, 8 ( H2 O)' _chemical_formula_sum 'C30 H46 N6 O16 Zn2' _chemical_formula_weight 877.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.247(3) _cell_length_b 9.8783(14) _cell_length_c 18.990(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.515(3) _cell_angle_gamma 90.00 _cell_volume 3756.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 106(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description poyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 1.356 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9016 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 106(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12811 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.09 _reflns_number_total 4146 _reflns_number_gt 2925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+10.6700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4146 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.626453(17) 0.43760(4) 0.70004(2) 0.01219(11) Uani 1 1 d . . . O1 O 0.62015(10) 0.2676(2) 0.76204(12) 0.0138(5) Uani 1 1 d . . . O2 O 0.59479(11) 0.0481(2) 0.76341(13) 0.0209(5) Uani 1 1 d . . . O3 O 0.30039(11) 0.5114(2) 0.20196(13) 0.0168(5) Uani 1 1 d . . . O4 O 0.20956(11) 0.3917(2) 0.14172(13) 0.0172(5) Uani 1 1 d . . . O5 O 0.67745(12) 0.3699(3) 0.63352(13) 0.0152(5) Uani 1 1 d . . . O6 O 0.20424(12) 0.5562(3) 0.37483(14) 0.0216(5) Uani 1 1 d . . . O7 O 0.31832(13) 0.7192(3) 0.07973(15) 0.0233(6) Uani 1 1 d . . . O8 O 0.21897(13) 0.5370(3) 0.01555(14) 0.0240(6) Uani 1 1 d . . . N1 N 0.54189(12) 0.5602(3) 0.67681(14) 0.0127(5) Uani 1 1 d . . . N2 N 0.53860(13) 0.3044(3) 0.62246(15) 0.0133(6) Uani 1 1 d . . . N3 N 0.33779(12) 0.3388(3) 0.31882(15) 0.0132(6) Uani 1 1 d . . . C1 C 0.54832(16) 0.6947(3) 0.68223(17) 0.0146(7) Uani 1 1 d . . . C2 C 0.49298(17) 0.7792(4) 0.66176(19) 0.0185(7) Uani 1 1 d . . . C3 C 0.43009(17) 0.7212(4) 0.63039(19) 0.0191(7) Uani 1 1 d . . . C4 C 0.42384(16) 0.5830(4) 0.62141(18) 0.0186(7) Uani 1 1 d . . . C5 C 0.48100(16) 0.5041(3) 0.64595(17) 0.0138(7) Uani 1 1 d . . . C6 C 0.48073(16) 0.3531(3) 0.64127(19) 0.0138(7) Uani 1 1 d . . . C7 C 0.53081(16) 0.3274(4) 0.54315(18) 0.0149(7) Uani 1 1 d . . . C8 C 0.46327(16) 0.3008(3) 0.49055(18) 0.0166(7) Uani 1 1 d . . . C9 C 0.40795(16) 0.2941(3) 0.44774(18) 0.0165(7) Uani 1 1 d . . . C10 C 0.34009(17) 0.2878(4) 0.39308(19) 0.0172(7) Uani 1 1 d . . . C11 C 0.38119(16) 0.2544(4) 0.2893(2) 0.0163(7) Uani 1 1 d . . . C12 C 0.55352(17) 0.1638(3) 0.64705(19) 0.0157(7) Uani 1 1 d . . . C13 C 0.59216(15) 0.1584(3) 0.73135(18) 0.0143(7) Uani 1 1 d . . . C14 C 0.26861(16) 0.3328(3) 0.26785(19) 0.0147(7) Uani 1 1 d . . . C15 C 0.25902(15) 0.4176(3) 0.19860(18) 0.0148(7) Uani 1 1 d . . . H51 H 0.687(2) 0.272(5) 0.636(2) 0.045(13) Uiso 1 1 d . . . H52 H 0.707(2) 0.401(4) 0.633(2) 0.028(14) Uiso 1 1 d . . . H61 H 0.215(2) 0.532(5) 0.431(3) 0.058(15) Uiso 1 1 d . . . H62 H 0.170(3) 0.509(5) 0.347(3) 0.057(16) Uiso 1 1 d . . . H71 H 0.341(3) 0.732(6) 0.136(4) 0.10(2) Uiso 1 1 d . . . H72 H 0.321(3) 0.799(6) 0.066(3) 0.067(18) Uiso 1 1 d . . . H81 H 0.258(2) 0.588(5) 0.044(3) 0.044(13) Uiso 1 1 d . . . H82 H 0.216(2) 0.482(5) 0.056(3) 0.058(15) Uiso 1 1 d . . . H2 H 0.4953(16) 0.868(4) 0.6680(18) 0.008(8) Uiso 1 1 d . . . H3 H 0.3972(18) 0.770(4) 0.617(2) 0.015(9) Uiso 1 1 d . . . H4 H 0.3771(18) 0.542(4) 0.598(2) 0.020(9) Uiso 1 1 d . . . H6A H 0.4415(17) 0.325(3) 0.603(2) 0.013(9) Uiso 1 1 d . . . H6B H 0.4844(15) 0.316(3) 0.6890(19) 0.008(8) Uiso 1 1 d . . . H7B H 0.5659(17) 0.267(4) 0.5278(19) 0.017(9) Uiso 1 1 d . . . H7A H 0.5423(17) 0.425(4) 0.536(2) 0.018(9) Uiso 1 1 d . . . H10A H 0.3286(15) 0.189(3) 0.3906(18) 0.007(8) Uiso 1 1 d . . . H10B H 0.3128(19) 0.342(4) 0.408(2) 0.024(10) Uiso 1 1 d . . . H11A H 0.3660(16) 0.268(3) 0.236(2) 0.011(8) Uiso 1 1 d . . . H11B H 0.3832(18) 0.160(4) 0.301(2) 0.020(10) Uiso 1 1 d . . . H12A H 0.5154(18) 0.104(4) 0.637(2) 0.017(9) Uiso 1 1 d . . . H12B H 0.5855(17) 0.124(4) 0.622(2) 0.017(9) Uiso 1 1 d . . . H14A H 0.2533(16) 0.239(3) 0.2527(18) 0.009(8) Uiso 1 1 d . . . H14B H 0.241(2) 0.374(4) 0.290(2) 0.031(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.00840(17) 0.01494(19) 0.01173(18) 0.00043(16) 0.00135(12) -0.00011(16) O1 0.0118(11) 0.0150(12) 0.0130(12) 0.0009(9) 0.0021(9) -0.0003(9) O2 0.0217(12) 0.0161(13) 0.0206(13) 0.0037(10) 0.0013(10) 0.0002(10) O3 0.0157(12) 0.0166(12) 0.0148(12) 0.0024(9) 0.0006(9) -0.0045(9) O4 0.0132(12) 0.0175(12) 0.0160(12) 0.0012(9) -0.0017(9) -0.0028(9) O5 0.0102(12) 0.0168(14) 0.0185(13) 0.0005(10) 0.0047(10) -0.0015(10) O6 0.0167(12) 0.0281(14) 0.0189(13) -0.0021(12) 0.0044(10) -0.0066(11) O7 0.0229(14) 0.0238(15) 0.0194(14) 0.0031(11) 0.0019(11) 0.0022(11) O8 0.0290(15) 0.0262(15) 0.0140(13) 0.0002(11) 0.0035(11) -0.0022(11) N1 0.0106(12) 0.0165(13) 0.0113(13) 0.0001(11) 0.0040(10) 0.0007(11) N2 0.0108(13) 0.0158(14) 0.0111(14) 0.0014(11) 0.0010(10) 0.0003(11) N3 0.0072(13) 0.0193(15) 0.0130(14) 0.0013(11) 0.0031(10) 0.0021(11) C1 0.0158(17) 0.0194(17) 0.0091(16) -0.0007(13) 0.0050(13) -0.0003(13) C2 0.0191(18) 0.021(2) 0.0155(18) -0.0010(14) 0.0060(14) 0.0058(14) C3 0.0159(18) 0.027(2) 0.0151(18) 0.0028(14) 0.0064(14) 0.0086(15) C4 0.0117(16) 0.029(2) 0.0154(17) 0.0015(14) 0.0045(13) 0.0029(14) C5 0.0117(16) 0.0224(17) 0.0082(16) -0.0003(13) 0.0045(12) -0.0003(13) C6 0.0084(16) 0.0207(18) 0.0111(17) 0.0022(13) 0.0017(13) -0.0025(13) C7 0.0123(16) 0.0178(18) 0.0122(17) -0.0004(13) 0.0011(12) -0.0012(13) C8 0.0163(17) 0.0195(17) 0.0128(17) 0.0022(13) 0.0031(13) 0.0014(14) C9 0.0185(18) 0.0184(18) 0.0130(17) 0.0025(13) 0.0058(14) -0.0007(14) C10 0.0142(17) 0.0219(19) 0.0129(17) 0.0043(14) 0.0011(13) -0.0032(14) C11 0.0138(17) 0.0169(18) 0.0169(19) 0.0003(14) 0.0036(13) -0.0005(13) C12 0.0155(17) 0.0131(17) 0.0160(17) 0.0006(13) 0.0017(13) -0.0023(13) C13 0.0092(15) 0.0186(17) 0.0144(17) -0.0007(13) 0.0029(12) 0.0008(13) C14 0.0100(16) 0.0155(17) 0.0161(17) 0.0010(13) 0.0011(13) -0.0032(13) C15 0.0127(15) 0.0140(17) 0.0162(16) -0.0017(13) 0.0027(12) 0.0034(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 2.033(2) . ? Zn1 O3 2.049(2) 5_666 ? Zn1 O1 2.081(2) . ? Zn1 N1 2.088(3) . ? Zn1 N2 2.356(3) . ? Zn1 N3 2.401(3) 5_666 ? O1 C13 1.275(4) . ? O2 C13 1.240(4) . ? O3 C15 1.264(4) . ? O3 Zn1 2.049(2) 5_666 ? O4 C15 1.256(4) . ? O5 H51 0.98(5) . ? O5 H52 0.70(4) . ? O6 H61 1.04(5) . ? O6 H62 0.88(5) . ? O7 H71 1.03(7) . ? O7 H72 0.84(6) . ? O8 H81 0.96(5) . ? O8 H82 0.96(5) . ? N1 C1 1.336(4) . ? N1 C5 1.348(4) . ? N2 C12 1.466(4) . ? N2 C6 1.471(4) . ? N2 C7 1.477(4) . ? N3 C14 1.466(4) . ? N3 C10 1.483(4) . ? N3 C11 1.485(4) . ? N3 Zn1 2.401(3) 5_666 ? C1 C2 1.388(5) . ? C1 C11 1.499(5) 5_666 ? C2 C3 1.392(5) . ? C2 H2 0.89(3) . ? C3 C4 1.376(5) . ? C3 H3 0.82(4) . ? C4 C5 1.386(5) . ? C4 H4 1.03(4) . ? C5 C6 1.495(5) . ? C6 H6A 0.94(3) . ? C6 H6B 0.96(3) . ? C7 C8 1.473(4) . ? C7 H7B 1.07(4) . ? C7 H7A 1.01(4) . ? C8 C9 1.187(4) . ? C9 C10 1.470(5) . ? C10 H10A 1.00(3) . ? C10 H10B 0.90(4) . ? C11 C1 1.499(4) 5_666 ? C11 H11A 0.97(3) . ? C11 H11B 0.96(4) . ? C12 C13 1.537(4) . ? C12 H12A 0.97(4) . ? C12 H12B 1.03(4) . ? C14 C15 1.515(5) . ? C14 H14A 0.99(3) . ? C14 H14B 0.94(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O3 104.19(10) . 5_666 ? O5 Zn1 O1 103.55(10) . . ? O3 Zn1 O1 81.79(9) 5_666 . ? O5 Zn1 N1 131.24(10) . . ? O3 Zn1 N1 112.80(10) 5_666 . ? O1 Zn1 N1 111.98(9) . . ? O5 Zn1 N2 84.43(10) . . ? O3 Zn1 N2 155.13(9) 5_666 . ? O1 Zn1 N2 73.48(9) . . ? N1 Zn1 N2 75.27(10) . . ? O5 Zn1 N3 87.09(10) . 5_666 ? O3 Zn1 N3 74.20(9) 5_666 5_666 ? O1 Zn1 N3 155.53(9) . 5_666 ? N1 Zn1 N3 74.20(9) . 5_666 ? N2 Zn1 N3 130.14(9) . 5_666 ? C13 O1 Zn1 122.2(2) . . ? C15 O3 Zn1 122.0(2) . 5_666 ? Zn1 O5 H51 116(3) . . ? Zn1 O5 H52 121(4) . . ? H51 O5 H52 106(4) . . ? H61 O6 H62 110(4) . . ? H71 O7 H72 99(5) . . ? H81 O8 H82 97(4) . . ? C1 N1 C5 120.0(3) . . ? C1 N1 Zn1 120.1(2) . . ? C5 N1 Zn1 119.1(2) . . ? C12 N2 C6 110.0(3) . . ? C12 N2 C7 114.2(3) . . ? C6 N2 C7 112.3(2) . . ? C12 N2 Zn1 106.76(19) . . ? C6 N2 Zn1 102.56(19) . . ? C7 N2 Zn1 110.31(19) . . ? C14 N3 C10 108.7(2) . . ? C14 N3 C11 109.9(3) . . ? C10 N3 C11 110.0(3) . . ? C14 N3 Zn1 103.65(19) . 5_666 ? C10 N3 Zn1 122.9(2) . 5_666 ? C11 N3 Zn1 101.10(18) . 5_666 ? N1 C1 C2 121.4(3) . . ? N1 C1 C11 115.2(3) . 5_666 ? C2 C1 C11 123.4(3) . 5_666 ? C1 C2 C3 118.3(3) . . ? C1 C2 H2 124(2) . . ? C3 C2 H2 118(2) . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 121(3) . . ? C2 C3 H3 119(3) . . ? C3 C4 C5 118.6(3) . . ? C3 C4 H4 119(2) . . ? C5 C4 H4 123(2) . . ? N1 C5 C4 121.4(3) . . ? N1 C5 C6 114.8(3) . . ? C4 C5 C6 123.8(3) . . ? N2 C6 C5 110.7(3) . . ? N2 C6 H6A 108(2) . . ? C5 C6 H6A 109(2) . . ? N2 C6 H6B 107.0(19) . . ? C5 C6 H6B 109(2) . . ? H6A C6 H6B 112(3) . . ? C8 C7 N2 114.6(3) . . ? C8 C7 H7B 109.0(19) . . ? N2 C7 H7B 109.9(19) . . ? C8 C7 H7A 108(2) . . ? N2 C7 H7A 109(2) . . ? H7B C7 H7A 106(3) . . ? C9 C8 C7 172.9(4) . . ? C8 C9 C10 178.3(4) . . ? C9 C10 N3 111.7(3) . . ? C9 C10 H10A 104.0(18) . . ? N3 C10 H10A 110.8(19) . . ? C9 C10 H10B 109(2) . . ? N3 C10 H10B 106(2) . . ? H10A C10 H10B 115(3) . . ? N3 C11 C1 110.3(3) . 5_666 ? N3 C11 H11A 106.6(19) . . ? C1 C11 H11A 105.8(19) 5_666 . ? N3 C11 H11B 116(2) . . ? C1 C11 H11B 106(2) 5_666 . ? H11A C11 H11B 111(3) . . ? N2 C12 C13 110.4(3) . . ? N2 C12 H12A 116(2) . . ? C13 C12 H12A 108(2) . . ? N2 C12 H12B 109(2) . . ? C13 C12 H12B 105(2) . . ? H12A C12 H12B 108(3) . . ? O2 C13 O1 125.5(3) . . ? O2 C13 C12 117.5(3) . . ? O1 C13 C12 116.9(3) . . ? N3 C14 C15 111.4(3) . . ? N3 C14 H14A 112.9(19) . . ? C15 C14 H14A 109.2(19) . . ? N3 C14 H14B 109(2) . . ? C15 C14 H14B 103(2) . . ? H14A C14 H14B 110(3) . . ? O4 C15 O3 124.1(3) . . ? O4 C15 C14 117.7(3) . . ? O3 C15 C14 118.2(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.09 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.794 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.097 #===END data_rs01 _database_code_depnum_ccdc_archive 'CCDC 247938' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H42 La2 N8 O20, 8(H2 O)' _chemical_formula_sum 'C30 H58 La2 N8 O28' _chemical_formula_weight 1256.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.3229(7) _cell_length_b 15.5290(11) _cell_length_c 31.113(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4504.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 1.976 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8241 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29931 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 32.02 _reflns_number_total 7531 _reflns_number_gt 5718 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+21.1300P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7531 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.544046(18) 0.487060(11) 0.147104(5) 0.00859(5) Uani 1 1 d . . . N1 N 0.3410(3) 0.44607(17) 0.08779(8) 0.0098(5) Uani 1 1 d . . . N2 N 0.6244(3) 0.39082(16) 0.06997(8) 0.0091(5) Uani 1 1 d . . . N3 N 0.6705(3) 0.38716(17) -0.12389(8) 0.0097(5) Uani 1 1 d . . . N4 N 0.7737(3) 0.58416(17) 0.09601(9) 0.0125(5) Uani 1 1 d . . . O1 O 0.6771(3) 0.34742(15) 0.15201(7) 0.0149(5) Uani 1 1 d . . . O2 O 0.8817(3) 0.27912(16) 0.13716(8) 0.0172(5) Uani 1 1 d . . . O3 O 0.6312(3) 0.46029(15) -0.20309(7) 0.0130(4) Uani 1 1 d . . . O4 O 0.6982(3) 0.34190(17) -0.23858(8) 0.0218(6) Uani 1 1 d . . . O5 O 0.8101(3) 0.52073(15) 0.11936(8) 0.0158(5) Uani 1 1 d . . . O6 O 0.6410(2) 0.59654(15) 0.08992(7) 0.0125(4) Uani 1 1 d . . . O7 O 0.8643(3) 0.63126(17) 0.07922(9) 0.0214(5) Uani 1 1 d . . . O8 O 0.6390(3) 0.62665(15) 0.17890(8) 0.0162(5) Uani 1 1 d . . . O9 O 0.6683(3) 0.46210(16) 0.21889(8) 0.0173(5) Uani 1 1 d . . . O10 O 0.3811(3) 0.36479(16) 0.17179(9) 0.0224(6) Uani 1 1 d . . . O11A O 0.8664(11) 0.3282(4) 0.2319(3) 0.073(3) Uani 0.615(9) 1 d P A 1 O12 O 0.9124(5) 0.3886(3) 0.32329(17) 0.0279(13) Uani 0.615(9) 1 d P A 1 O11B O 0.8182(7) 0.3359(4) 0.2608(3) 0.0178(17) Uani 0.385(9) 1 d P A 2 O13 O 0.5258(4) 0.2290(2) 0.20611(13) 0.0452(10) Uani 1 1 d . . . O14 O 0.5279(4) 0.0475(3) 0.20783(13) 0.0477(10) Uani 1 1 d . . . C1 C 0.2164(3) 0.4893(2) 0.08563(10) 0.0112(5) Uani 1 1 d . . . C2 C 0.1082(3) 0.4672(2) 0.05673(11) 0.0144(6) Uani 1 1 d . . . H2 H 0.0195 0.4974 0.0567 0.014(6) Uiso 1 1 calc R . . C3 C 0.1321(4) 0.4005(2) 0.02805(11) 0.0145(6) Uani 1 1 d . . . H3 H 0.0605 0.3848 0.0078 0.014(6) Uiso 1 1 calc R . . C4 C 0.2620(4) 0.3568(2) 0.02928(11) 0.0136(6) Uani 1 1 d . . . H4 H 0.2820 0.3121 0.0093 0.014(6) Uiso 1 1 calc R . . C5 C 0.3626(3) 0.37980(19) 0.06038(10) 0.0096(5) Uani 1 1 d . . . C6 C 0.5009(3) 0.3315(2) 0.06555(10) 0.0115(6) Uani 1 1 d . . . H6A H 0.4950 0.2943 0.0913 0.014(3) Uiso 1 1 calc R . . H6B H 0.5158 0.2939 0.0402 0.014(3) Uiso 1 1 calc R . . C7 C 0.6412(4) 0.44366(19) 0.03067(9) 0.0108(5) Uani 1 1 d . . . H7A H 0.5610 0.4854 0.0295 0.014(3) Uiso 1 1 calc R . . H7B H 0.7311 0.4772 0.0332 0.014(3) Uiso 1 1 calc R . . C8 C 0.6449(4) 0.3963(2) -0.01008(10) 0.0119(6) Uani 1 1 d . . . C9 C 0.6456(4) 0.3645(2) -0.04526(10) 0.0117(6) Uani 1 1 d . . . C10 C 0.6491(4) 0.3248(2) -0.08820(10) 0.0121(6) Uani 1 1 d . . . H10A H 0.5578 0.2937 -0.0930 0.014(3) Uiso 1 1 calc R . . H10B H 0.7276 0.2819 -0.0890 0.014(3) Uiso 1 1 calc R . . C11 C 0.8041(3) 0.4377(2) -0.11710(11) 0.0130(6) Uani 1 1 d . . . H11A H 0.8364 0.4614 -0.1450 0.014(3) Uiso 1 1 calc R . . H11B H 0.8802 0.3989 -0.1063 0.014(3) Uiso 1 1 calc R . . C12 C 0.7562(3) 0.3415(2) 0.07887(10) 0.0118(6) Uani 1 1 d . . . H12A H 0.8404 0.3753 0.0692 0.014(3) Uiso 1 1 calc R . . H12B H 0.7542 0.2872 0.0622 0.014(3) Uiso 1 1 calc R . . C13 C 0.7726(4) 0.32057(19) 0.12649(10) 0.0121(6) Uani 1 1 d . . . C15 C 0.6721(4) 0.3825(2) -0.20481(10) 0.0135(6) Uani 1 1 d . . . C14 C 0.6908(4) 0.3335(2) -0.16299(10) 0.0136(6) Uani 1 1 d . . . H14A H 0.6211 0.2854 -0.1623 0.014(3) Uiso 1 1 calc R . . H14B H 0.7883 0.3082 -0.1623 0.014(3) Uiso 1 1 calc R . . H81 H 0.6603 0.6337 0.2053 0.043(6) Uiso 1 1 d . . . H82 H 0.6134 0.6743 0.1688 0.043(6) Uiso 1 1 d . . . H91 H 0.7131 0.4178 0.2234 0.043(6) Uiso 1 1 d . . . H92 H 0.6570 0.4813 0.2410 0.043(6) Uiso 1 1 d . . . H101 H 0.4154 0.3195 0.1784 0.043(6) Uiso 1 1 d . . . H102 H 0.3093 0.3703 0.1827 0.043(6) Uiso 1 1 d . . . H141 H 0.5316 0.1012 0.2018 0.043(6) Uiso 1 1 d . . . H142 H 0.6097 0.0376 0.1946 0.043(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01020(7) 0.00888(7) 0.00669(8) -0.00011(6) -0.00053(6) 0.00034(6) N1 0.0111(11) 0.0120(12) 0.0062(12) 0.0004(9) 0.0010(9) -0.0009(9) N2 0.0106(11) 0.0108(11) 0.0060(12) 0.0009(8) -0.0010(9) 0.0014(9) N3 0.0137(12) 0.0113(12) 0.0040(12) -0.0005(8) 0.0004(9) 0.0006(9) N4 0.0134(12) 0.0123(12) 0.0118(13) -0.0028(9) 0.0010(10) -0.0007(10) O1 0.0211(12) 0.0160(11) 0.0077(11) 0.0003(8) 0.0027(9) 0.0065(9) O2 0.0195(12) 0.0168(11) 0.0153(12) 0.0002(8) -0.0052(9) 0.0061(9) O3 0.0156(11) 0.0142(10) 0.0092(11) 0.0013(8) 0.0013(9) 0.0023(9) O4 0.0343(15) 0.0232(13) 0.0080(12) -0.0009(9) -0.0001(10) 0.0102(11) O5 0.0162(11) 0.0147(11) 0.0167(12) 0.0023(9) -0.0012(9) 0.0017(9) O6 0.0107(10) 0.0174(11) 0.0095(11) -0.0003(8) 0.0006(8) 0.0006(8) O7 0.0164(12) 0.0210(12) 0.0269(14) 0.0042(10) 0.0035(11) -0.0042(10) O8 0.0257(13) 0.0136(11) 0.0093(11) 0.0004(8) -0.0022(10) -0.0034(9) O9 0.0260(13) 0.0186(11) 0.0075(11) -0.0023(8) -0.0049(9) 0.0074(10) O10 0.0227(13) 0.0140(11) 0.0303(15) 0.0023(10) 0.0072(11) -0.0017(10) O11A 0.101(7) 0.035(3) 0.082(7) -0.020(4) -0.067(6) 0.026(4) O12 0.024(2) 0.026(2) 0.034(3) 0.006(2) -0.001(2) -0.0006(18) O11B 0.020(3) 0.011(3) 0.022(4) 0.006(3) 0.006(3) 0.006(2) O13 0.0291(18) 0.054(2) 0.052(2) 0.0294(19) 0.0013(16) 0.0034(15) O14 0.0327(19) 0.061(2) 0.049(2) -0.0288(19) 0.0127(17) -0.0138(17) C1 0.0112(12) 0.0132(13) 0.0094(14) -0.0003(10) 0.0004(10) -0.0004(11) C2 0.0106(14) 0.0190(15) 0.0135(15) -0.0004(11) -0.0018(11) -0.0001(11) C3 0.0143(14) 0.0181(15) 0.0110(15) -0.0011(11) -0.0025(12) -0.0038(12) C4 0.0157(14) 0.0149(14) 0.0100(15) -0.0017(11) -0.0001(12) -0.0019(11) C5 0.0110(13) 0.0099(13) 0.0079(13) 0.0012(10) 0.0018(11) -0.0018(10) C6 0.0133(13) 0.0114(13) 0.0097(14) -0.0007(10) 0.0003(11) -0.0011(10) C7 0.0164(14) 0.0107(13) 0.0054(13) 0.0006(9) 0.0007(11) 0.0004(11) C8 0.0159(14) 0.0127(14) 0.0069(14) 0.0021(10) 0.0005(11) -0.0003(11) C9 0.0161(14) 0.0126(14) 0.0063(14) 0.0015(10) 0.0000(11) 0.0017(11) C10 0.0185(15) 0.0133(14) 0.0046(13) 0.0017(10) 0.0000(11) 0.0036(11) C11 0.0104(13) 0.0170(15) 0.0116(15) -0.0038(11) 0.0008(11) 0.0013(11) C12 0.0119(13) 0.0130(14) 0.0104(14) -0.0004(10) 0.0009(11) 0.0028(11) C13 0.0191(15) 0.0084(13) 0.0090(14) 0.0007(10) -0.0024(11) 0.0008(11) C15 0.0154(14) 0.0177(15) 0.0074(14) 0.0013(11) -0.0001(11) 0.0012(11) C14 0.0207(16) 0.0134(14) 0.0067(14) -0.0025(10) -0.0017(12) 0.0033(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O1 2.503(2) . ? La1 O3 2.524(2) 5_665 ? La1 O8 2.542(2) . ? La1 O9 2.546(2) . ? La1 O10 2.550(3) . ? La1 O6 2.622(2) . ? La1 O5 2.678(3) . ? La1 N1 2.719(3) . ? La1 N3 2.888(3) 5_665 ? La1 N2 2.925(3) . ? La1 N4 3.063(3) . ? N1 C1 1.343(4) . ? N1 C5 1.352(4) . ? N2 C12 1.474(4) . ? N2 C7 1.481(4) . ? N2 C6 1.482(4) . ? N3 C10 1.486(4) . ? N3 C11 1.486(4) . ? N3 C14 1.487(4) . ? N3 La1 2.888(3) 5_665 ? N4 O7 1.233(4) . ? N4 O6 1.266(4) . ? N4 O5 1.270(4) . ? O1 C13 1.264(4) . ? O2 C13 1.248(4) . ? O3 C15 1.268(4) . ? O3 La1 2.524(2) 5_665 ? O4 C15 1.249(4) . ? O8 H81 0.85 . ? O8 H82 0.84 . ? O9 H91 0.82 . ? O9 H92 0.76 . ? O10 H101 0.80 . ? O10 H102 0.76 . ? O14 H141 0.86 . ? O14 H142 0.88 . ? C1 C2 1.395(4) . ? C1 C11 1.511(5) 5_665 ? C2 C3 1.385(5) . ? C2 H2 0.9500 . ? C3 C4 1.389(5) . ? C3 H3 0.9500 . ? C4 C5 1.394(4) . ? C4 H4 0.9500 . ? C5 C6 1.500(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.466(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.200(4) . ? C9 C10 1.472(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C1 1.511(5) 5_665 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.525(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C15 C14 1.517(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 La1 O3 124.01(7) . 5_665 ? O1 La1 O8 122.84(8) . . ? O3 La1 O8 71.38(8) 5_665 . ? O1 La1 O9 65.73(8) . . ? O3 La1 O9 74.84(8) 5_665 . ? O8 La1 O9 68.28(8) . . ? O1 La1 O10 68.40(8) . . ? O3 La1 O10 69.38(8) 5_665 . ? O8 La1 O10 136.49(9) . . ? O9 La1 O10 83.88(9) . . ? O1 La1 O6 115.61(8) . . ? O3 La1 O6 118.78(7) 5_665 . ? O8 La1 O6 65.85(7) . . ? O9 La1 O6 122.49(8) . . ? O10 La1 O6 153.21(9) . . ? O1 La1 O5 74.31(8) . . ? O3 La1 O5 139.35(8) 5_665 . ? O8 La1 O5 68.67(8) . . ? O9 La1 O5 83.74(8) . . ? O10 La1 O5 142.58(8) . . ? O6 La1 O5 48.34(7) . . ? O1 La1 N1 100.59(8) . . ? O3 La1 N1 95.36(8) 5_665 . ? O8 La1 N1 134.93(8) . . ? O9 La1 N1 151.23(8) . . ? O10 La1 N1 67.38(9) . . ? O6 La1 N1 86.06(7) . . ? O5 La1 N1 118.15(8) . . ? O1 La1 N3 160.85(8) . 5_665 ? O3 La1 N3 60.33(7) 5_665 5_665 ? O8 La1 N3 76.22(8) . 5_665 ? O9 La1 N3 129.62(8) . 5_665 ? O10 La1 N3 99.57(8) . 5_665 ? O6 La1 N3 68.32(7) . 5_665 ? O5 La1 N3 115.41(7) . 5_665 ? N1 La1 N3 60.41(8) . 5_665 ? O1 La1 N2 58.69(7) . . ? O3 La1 N2 153.83(8) 5_665 . ? O8 La1 N2 131.74(8) . . ? O9 La1 N2 121.70(8) . . ? O10 La1 N2 91.11(8) . . ? O6 La1 N2 71.71(7) . . ? O5 La1 N2 66.29(7) . . ? N1 La1 N2 60.13(8) . . ? N3 La1 N2 108.53(7) 5_665 . ? O1 La1 N4 96.41(8) . . ? O3 La1 N4 130.62(7) 5_665 . ? O8 La1 N4 62.53(8) . . ? O9 La1 N4 102.25(8) . . ? O10 La1 N4 159.90(8) . . ? O6 La1 N4 24.17(7) . . ? O5 La1 N4 24.39(7) . . ? N1 La1 N4 104.46(8) . . ? N3 La1 N4 91.23(7) 5_665 . ? N2 La1 N4 69.31(7) . . ? C1 N1 C5 118.5(3) . . ? C1 N1 La1 121.3(2) . . ? C5 N1 La1 120.2(2) . . ? C12 N2 C7 110.8(2) . . ? C12 N2 C6 110.0(2) . . ? C7 N2 C6 110.5(2) . . ? C12 N2 La1 108.95(18) . . ? C7 N2 La1 114.92(17) . . ? C6 N2 La1 101.24(17) . . ? C10 N3 C11 110.5(3) . . ? C10 N3 C14 105.3(2) . . ? C11 N3 C14 107.8(2) . . ? C10 N3 La1 122.29(19) . 5_665 ? C11 N3 La1 105.00(18) . 5_665 ? C14 N3 La1 105.21(18) . 5_665 ? O7 N4 O6 121.0(3) . . ? O7 N4 O5 121.3(3) . . ? O6 N4 O5 117.7(3) . . ? O7 N4 La1 172.0(2) . . ? O6 N4 La1 57.96(15) . . ? O5 N4 La1 60.55(16) . . ? C13 O1 La1 126.6(2) . . ? C15 O3 La1 122.2(2) . 5_665 ? N4 O5 La1 95.05(18) . . ? N4 O6 La1 97.87(18) . . ? La1 O8 H81 124 . . ? La1 O8 H82 120 . . ? H81 O8 H82 108 . . ? La1 O9 H91 121 . . ? La1 O9 H92 132 . . ? H91 O9 H92 104 . . ? La1 O10 H101 120 . . ? La1 O10 H102 125 . . ? H101 O10 H102 110 . . ? H141 O14 H142 92 . . ? N1 C1 C2 122.4(3) . . ? N1 C1 C11 116.9(3) . 5_665 ? C2 C1 C11 120.7(3) . 5_665 ? C3 C2 C1 118.9(3) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.2(3) . . ? N1 C5 C6 116.2(3) . . ? C4 C5 C6 121.6(3) . . ? N2 C6 C5 111.5(2) . . ? N2 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C8 C7 N2 116.0(3) . . ? C8 C7 H7A 108.3 . . ? N2 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? N2 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C9 C8 C7 174.0(3) . . ? C8 C9 C10 178.9(4) . . ? C9 C10 N3 114.1(3) . . ? C9 C10 H10A 108.7 . . ? N3 C10 H10A 108.7 . . ? C9 C10 H10B 108.7 . . ? N3 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N3 C11 C1 112.5(3) . 5_665 ? N3 C11 H11A 109.1 . . ? C1 C11 H11A 109.1 5_665 . ? N3 C11 H11B 109.1 . . ? C1 C11 H11B 109.1 5_665 . ? H11A C11 H11B 107.8 . . ? N2 C12 C13 112.2(3) . . ? N2 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? N2 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? O2 C13 O1 125.2(3) . . ? O2 C13 C12 116.8(3) . . ? O1 C13 C12 118.0(3) . . ? O4 C15 O3 125.1(3) . . ? O4 C15 C14 116.5(3) . . ? O3 C15 C14 118.4(3) . . ? N3 C14 C15 114.0(3) . . ? N3 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? N3 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 32.02 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 2.480 _refine_diff_density_min -1.732 _refine_diff_density_rms 0.153 #===END data_rs02 _database_code_depnum_ccdc_archive 'CCDC 247939' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H43 Eu2 N6 Na1.50 O17' _chemical_formula_sum 'C36 H43 Eu2 N6 Na1.50 O17' _chemical_formula_weight 1170.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3530(5) _cell_length_b 13.0001(6) _cell_length_c 18.6967(8) _cell_angle_alpha 91.0640(10) _cell_angle_beta 103.0820(10) _cell_angle_gamma 93.9490(10) _cell_volume 2443.75(19) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1159 _exptl_absorpt_coefficient_mu 2.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8596 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42904 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 32.01 _reflns_number_total 16591 _reflns_number_gt 14645 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; There is a disordered region in the cell (volume ca 450 A3) which could not be described satisfactorily. Therefor a correction by SQUEEZE (PLATON, A.Spek) was used (165 electrons). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+3.6700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16591 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.845633(10) 0.310682(8) 0.224483(6) 0.01455(3) Uani 1 1 d . . . Eu2 Eu 0.872170(10) 0.668033(8) 0.180186(6) 0.01363(3) Uani 1 1 d . . . Na2 Na 0.81606(11) 1.08688(10) 0.08297(6) 0.0272(2) Uani 1 1 d . . . Na1 Na 0.5000 0.0000 0.0000 0.0150(2) Uani 1 2 d S . . O1 O 0.9530(2) 0.16228(14) 0.20381(12) 0.0271(4) Uani 1 1 d . . . O2 O 1.1397(3) 0.0820(2) 0.21372(18) 0.0584(9) Uani 1 1 d . . . O3 O 1.03417(18) 0.74906(15) 0.12277(10) 0.0212(3) Uani 1 1 d . . . O4 O 1.23731(19) 0.74166(17) 0.10262(11) 0.0273(4) Uani 1 1 d . . . O5 O 0.79230(18) 0.80993(14) 0.11406(11) 0.0213(3) Uani 1 1 d . . . O6 O 0.67024(19) 0.94552(14) 0.09559(10) 0.0227(3) Uani 1 1 d . . . O7 O 0.69406(18) 0.19882(15) 0.13871(10) 0.0229(4) Uani 1 1 d . . . O8 O 0.4908(2) 0.15737(15) 0.06832(11) 0.0241(4) Uani 1 1 d . . . O9 O 0.72589(19) 0.57222(14) 0.08194(12) 0.0256(4) Uani 1 1 d . . . O10 O 0.73925(19) 0.43288(19) 0.14726(11) 0.0288(4) Uani 1 1 d . . . O11 O 1.0100(2) 0.37052(19) 0.1636(2) 0.0560(9) Uani 1 1 d . . . O12 O 1.0045(2) 0.53797(16) 0.15766(13) 0.0296(4) Uani 1 1 d . . . O13 O 0.84762(17) 0.43294(14) 0.31662(10) 0.0194(3) Uani 1 1 d . . . O14 O 0.85675(17) 0.59834(14) 0.29131(10) 0.0187(3) Uani 1 1 d . . . O15 O 0.6871(2) 1.07006(18) -0.04400(13) 0.0270(4) Uani 1 1 d . . . O16 O 0.9245(3) 1.2287(3) 0.03718(14) 0.0458(7) Uani 1 1 d . . . O17 O 0.0808(6) 0.1537(5) -0.0274(3) 0.1089(17) Uiso 1 1 d . . . N1 N 0.8289(2) 0.22804(16) 0.34765(12) 0.0200(4) Uani 1 1 d . . . N2 N 1.0776(2) 0.29058(15) 0.32600(12) 0.0196(4) Uani 1 1 d . . . N3 N 1.11029(19) 0.72707(15) 0.26712(11) 0.0150(3) Uani 1 1 d . . . N4 N 0.8697(2) 0.80886(16) 0.27772(13) 0.0196(4) Uani 1 1 d . . . N5 N 0.6263(2) 0.71478(16) 0.19593(13) 0.0193(4) Uani 1 1 d . . . N6 N 0.5998(2) 0.27990(16) 0.24758(11) 0.0173(4) Uani 1 1 d . . . C1 C 0.7101(3) 0.18819(18) 0.35535(13) 0.0195(4) Uani 1 1 d . . . C2 C 0.6859(3) 0.15960(19) 0.42219(14) 0.0230(5) Uani 1 1 d . . . H2 H 0.6003 0.1319 0.4257 0.035(4) Uiso 1 1 calc R . . C3 C 0.7895(3) 0.1722(2) 0.48406(14) 0.0253(5) Uani 1 1 d . . . H3 H 0.7766 0.1516 0.5306 0.035(4) Uiso 1 1 calc R . . C4 C 0.9112(3) 0.2150(2) 0.47721(14) 0.0242(5) Uani 1 1 d . . . H4 H 0.9832 0.2246 0.5190 0.035(4) Uiso 1 1 calc R . . C5 C 0.9279(3) 0.24417(18) 0.40813(14) 0.0206(4) Uani 1 1 d . . . C6 C 1.0553(3) 0.30130(19) 0.40043(14) 0.0222(5) Uani 1 1 d . . . H6A H 1.0526 0.3754 0.4129 0.029(2) Uiso 1 1 calc R . . H6B H 1.1308 0.2747 0.4358 0.029(2) Uiso 1 1 calc R . . C7 C 1.1902(2) 0.36515(19) 0.31891(16) 0.0230(5) Uani 1 1 d . . . H7A H 1.2698 0.3509 0.3569 0.029(2) Uiso 1 1 calc R . . H7B H 1.2105 0.3528 0.2704 0.029(2) Uiso 1 1 calc R . . C8 C 1.1656(2) 0.47439(19) 0.32615(13) 0.0180(4) Uani 1 1 d . . . C9 C 1.1569(2) 0.56516(18) 0.33139(12) 0.0162(4) Uani 1 1 d . . . C10 C 1.1510(2) 0.67707(18) 0.33892(12) 0.0163(4) Uani 1 1 d . . . H10A H 1.2395 0.7081 0.3650 0.029(2) Uiso 1 1 calc R . . H10B H 1.0870 0.6914 0.3694 0.029(2) Uiso 1 1 calc R . . C11 C 1.1044(2) 0.83931(18) 0.28144(14) 0.0193(4) Uani 1 1 d . . . H11A H 1.1021 0.8761 0.2353 0.029(2) Uiso 1 1 calc R . . H11B H 1.1859 0.8655 0.3177 0.029(2) Uiso 1 1 calc R . . C12 C 0.9850(2) 0.86219(18) 0.31006(14) 0.0185(4) Uani 1 1 d . . . C13 C 0.9935(3) 0.93438(19) 0.36690(16) 0.0241(5) Uani 1 1 d . . . H13 H 1.0763 0.9697 0.3900 0.035(4) Uiso 1 1 calc R . . C14 C 0.8786(3) 0.9536(2) 0.3891(2) 0.0370(7) Uani 1 1 d . . . H14 H 0.8810 1.0041 0.4268 0.035(4) Uiso 1 1 calc R . . C15 C 0.7599(3) 0.8986(3) 0.3561(2) 0.0432(9) Uani 1 1 d . . . H15 H 0.6802 0.9113 0.3707 0.035(4) Uiso 1 1 calc R . . C16 C 0.7592(3) 0.8249(2) 0.30145(17) 0.0260(5) Uani 1 1 d . . . C17 C 0.6379(2) 0.7526(2) 0.27227(17) 0.0256(5) Uani 1 1 d . . . H17A H 0.6407 0.6926 0.3043 0.029(2) Uiso 1 1 calc R . . H17B H 0.5577 0.7885 0.2747 0.029(2) Uiso 1 1 calc R . . C18 C 0.5201(2) 0.62830(18) 0.17863(14) 0.0180(4) Uani 1 1 d . . . H18A H 0.4347 0.6558 0.1818 0.029(2) Uiso 1 1 calc R . . H18B H 0.5115 0.6042 0.1271 0.029(2) Uiso 1 1 calc R . . C19 C 0.5401(2) 0.53940(19) 0.22533(13) 0.0173(4) Uani 1 1 d . . . C20 C 0.5442(2) 0.4597(2) 0.25672(13) 0.0193(4) Uani 1 1 d . . . C21 C 0.5519(2) 0.3596(2) 0.29164(13) 0.0193(4) Uani 1 1 d . . . H21A H 0.4627 0.3356 0.2984 0.029(2) Uiso 1 1 calc R . . H21B H 0.6128 0.3681 0.3408 0.029(2) Uiso 1 1 calc R . . C22 C 0.6021(3) 0.1810(2) 0.28637(14) 0.0218(5) Uani 1 1 d . . . H22A H 0.6174 0.1245 0.2537 0.029(2) Uiso 1 1 calc R . . H22B H 0.5151 0.1648 0.2987 0.029(2) Uiso 1 1 calc R . . C23 C 1.1188(3) 0.18543(19) 0.31522(17) 0.0260(5) Uani 1 1 d . . . H23A H 1.0859 0.1389 0.3496 0.029(3) Uiso 1 1 calc R . . H23B H 1.2171 0.1876 0.3277 0.029(3) Uiso 1 1 calc R . . C24 C 1.0680(3) 0.1411(2) 0.23785(18) 0.0313(6) Uani 1 1 d . . . C25 C 1.2105(2) 0.71393(19) 0.22341(13) 0.0174(4) Uani 1 1 d . . . H25A H 1.2372 0.6422 0.2270 0.029(3) Uiso 1 1 calc R . . H25B H 1.2904 0.7607 0.2439 0.029(3) Uiso 1 1 calc R . . C26 C 1.1575(2) 0.73687(19) 0.14322(14) 0.0193(4) Uani 1 1 d . . . C27 C 0.5804(3) 0.7970(2) 0.1436(2) 0.0302(6) Uani 1 1 d . . . H27A H 0.5330 0.8458 0.1677 0.029(3) Uiso 1 1 calc R . . H27B H 0.5158 0.7647 0.1004 0.029(3) Uiso 1 1 calc R . . C28 C 0.6897(2) 0.85731(19) 0.11700(14) 0.0195(4) Uani 1 1 d . . . C29 C 0.5077(2) 0.2636(2) 0.17501(13) 0.0205(4) Uani 1 1 d . . . H29A H 0.4865 0.3313 0.1538 0.029(3) Uiso 1 1 calc R . . H29B H 0.4237 0.2271 0.1808 0.029(3) Uiso 1 1 calc R . . C30 C 0.5674(2) 0.20070(19) 0.12280(13) 0.0193(4) Uani 1 1 d . . . C31 C 0.7062(2) 0.47668(18) 0.08742(12) 0.0154(4) Uani 1 1 d . . . C32 C 0.6387(3) 0.4128(2) 0.02015(15) 0.0288(6) Uani 1 1 d . . . H32A H 0.6907 0.3540 0.0151 0.063(5) Uiso 1 1 calc R . . H32B H 0.6317 0.4550 -0.0233 0.063(5) Uiso 1 1 calc R . . H32C H 0.5495 0.3876 0.0245 0.063(5) Uiso 1 1 calc R . . C33 C 1.0451(3) 0.4569(2) 0.14260(17) 0.0273(6) Uani 1 1 d . . . C34 C 1.1496(8) 0.4561(4) 0.0990(5) 0.124(4) Uani 1 1 d . . . H34A H 1.1226 0.4958 0.0547 0.063(5) Uiso 1 1 calc R . . H34B H 1.1606 0.3849 0.0848 0.063(5) Uiso 1 1 calc R . . H34C H 1.2340 0.4872 0.1288 0.063(5) Uiso 1 1 calc R . . C35 C 0.8497(2) 0.52604(18) 0.33365(12) 0.0154(4) Uani 1 1 d . . . C36 C 0.8460(4) 0.5533(3) 0.41181(16) 0.0406(8) Uani 1 1 d . . . H36A H 0.9365 0.5574 0.4426 0.063(5) Uiso 1 1 calc R . . H36B H 0.7908 0.5001 0.4299 0.063(5) Uiso 1 1 calc R . . H36C H 0.8082 0.6201 0.4137 0.063(5) Uiso 1 1 calc R . . H161 H 0.978(6) 1.241(5) 0.038(4) 0.07(2) Uiso 1 1 d . . . H151 H 0.709(4) 1.115(4) -0.066(2) 0.036(11) Uiso 1 1 d . . . H152 H 0.710(5) 1.027(4) -0.053(3) 0.040(13) Uiso 1 1 d . . . H162 H 0.900(5) 1.239(4) -0.014(3) 0.046(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01148(5) 0.01610(5) 0.01502(5) 0.00471(4) 0.00090(4) -0.00025(4) Eu2 0.00903(5) 0.01406(5) 0.01665(5) 0.00183(4) 0.00043(4) 0.00083(4) Na2 0.0167(5) 0.0423(7) 0.0248(5) 0.0127(5) 0.0067(4) 0.0077(4) Na1 0.0136(6) 0.0141(6) 0.0161(6) 0.0014(4) 0.0006(5) 0.0019(4) O1 0.0289(10) 0.0148(8) 0.0309(10) 0.0026(7) -0.0081(8) 0.0030(7) O2 0.0593(18) 0.0393(14) 0.0617(18) -0.0224(13) -0.0241(14) 0.0337(13) O3 0.0143(7) 0.0278(9) 0.0218(8) 0.0104(7) 0.0034(6) 0.0042(6) O4 0.0170(8) 0.0384(11) 0.0287(9) 0.0171(8) 0.0083(7) 0.0031(7) O5 0.0190(8) 0.0177(8) 0.0263(9) 0.0046(6) 0.0012(7) 0.0061(6) O6 0.0230(9) 0.0178(8) 0.0243(9) 0.0031(6) -0.0022(7) 0.0058(7) O7 0.0168(8) 0.0284(9) 0.0213(8) -0.0035(7) 0.0015(7) -0.0030(7) O8 0.0227(9) 0.0214(9) 0.0238(9) -0.0061(7) -0.0036(7) 0.0016(7) O9 0.0186(8) 0.0170(8) 0.0357(10) -0.0034(7) -0.0054(7) 0.0027(6) O10 0.0181(8) 0.0504(13) 0.0210(9) 0.0165(8) 0.0064(7) 0.0138(8) O11 0.0271(11) 0.0281(11) 0.128(3) 0.0412(15) 0.0423(15) 0.0144(9) O12 0.0175(8) 0.0215(9) 0.0454(12) -0.0077(8) -0.0029(8) 0.0058(7) O13 0.0155(7) 0.0183(8) 0.0214(8) 0.0031(6) -0.0012(6) -0.0020(6) O14 0.0146(7) 0.0179(8) 0.0232(8) 0.0039(6) 0.0033(6) -0.0002(6) O15 0.0239(9) 0.0226(10) 0.0378(11) 0.0053(8) 0.0140(8) 0.0006(8) O16 0.0270(12) 0.083(2) 0.0233(11) 0.0145(12) 0.0018(9) -0.0127(13) N1 0.0217(10) 0.0167(9) 0.0179(9) 0.0046(7) -0.0014(7) -0.0053(7) N2 0.0152(9) 0.0128(8) 0.0272(10) 0.0054(7) -0.0021(8) -0.0011(7) N3 0.0120(8) 0.0134(8) 0.0193(8) 0.0046(6) 0.0026(7) -0.0001(6) N4 0.0138(9) 0.0143(8) 0.0285(10) -0.0016(7) 0.0010(8) 0.0001(7) N5 0.0110(8) 0.0151(9) 0.0303(10) -0.0004(7) 0.0018(7) 0.0000(7) N6 0.0148(8) 0.0193(9) 0.0162(8) 0.0015(7) 0.0011(7) -0.0019(7) C1 0.0213(11) 0.0163(10) 0.0187(10) 0.0029(8) 0.0017(8) -0.0051(8) C2 0.0305(13) 0.0175(10) 0.0210(11) 0.0019(8) 0.0075(10) -0.0037(9) C3 0.0364(14) 0.0232(12) 0.0166(10) 0.0021(8) 0.0067(10) 0.0023(10) C4 0.0331(14) 0.0193(11) 0.0167(10) 0.0010(8) -0.0012(9) 0.0004(10) C5 0.0234(11) 0.0150(10) 0.0197(10) 0.0048(8) -0.0026(9) -0.0011(8) C6 0.0201(11) 0.0187(10) 0.0219(11) 0.0069(8) -0.0066(9) -0.0031(8) C7 0.0112(9) 0.0175(10) 0.0369(14) 0.0051(9) -0.0018(9) 0.0002(8) C8 0.0113(9) 0.0213(10) 0.0188(10) 0.0058(8) -0.0015(8) -0.0012(8) C9 0.0116(9) 0.0201(10) 0.0154(9) 0.0058(7) 0.0001(7) -0.0014(7) C10 0.0129(9) 0.0168(9) 0.0167(9) 0.0024(7) -0.0012(7) -0.0015(7) C11 0.0152(10) 0.0127(9) 0.0280(11) 0.0021(8) 0.0016(9) -0.0027(7) C12 0.0147(10) 0.0127(9) 0.0256(11) 0.0014(8) -0.0006(8) -0.0002(7) C13 0.0210(11) 0.0148(10) 0.0327(13) -0.0037(9) -0.0004(10) -0.0011(8) C14 0.0256(14) 0.0278(14) 0.054(2) -0.0241(13) 0.0052(13) -0.0007(11) C15 0.0198(13) 0.0361(17) 0.071(2) -0.0343(17) 0.0091(14) -0.0010(11) C16 0.0153(10) 0.0187(11) 0.0419(15) -0.0135(10) 0.0038(10) 0.0004(8) C17 0.0139(10) 0.0233(12) 0.0384(14) -0.0156(10) 0.0052(10) -0.0008(9) C18 0.0087(9) 0.0194(10) 0.0246(11) -0.0030(8) 0.0018(8) -0.0001(7) C19 0.0115(9) 0.0228(11) 0.0175(9) -0.0059(8) 0.0045(8) -0.0002(8) C20 0.0131(9) 0.0249(11) 0.0193(10) -0.0033(8) 0.0034(8) -0.0018(8) C21 0.0143(10) 0.0255(11) 0.0177(10) 0.0001(8) 0.0041(8) -0.0029(8) C22 0.0204(11) 0.0210(11) 0.0217(11) 0.0042(8) 0.0022(9) -0.0070(9) C23 0.0220(12) 0.0141(10) 0.0368(14) 0.0059(9) -0.0048(10) 0.0034(9) C24 0.0303(14) 0.0155(11) 0.0405(16) 0.0002(10) -0.0093(12) 0.0067(10) C25 0.0109(9) 0.0201(10) 0.0208(10) 0.0075(8) 0.0029(8) 0.0003(7) C26 0.0161(10) 0.0185(10) 0.0233(11) 0.0098(8) 0.0037(8) 0.0017(8) C27 0.0122(10) 0.0197(11) 0.0552(18) 0.0116(11) -0.0008(11) 0.0027(9) C28 0.0151(10) 0.0172(10) 0.0217(10) 0.0001(8) -0.0053(8) 0.0021(8) C29 0.0140(10) 0.0261(12) 0.0186(10) -0.0015(8) -0.0009(8) -0.0027(8) C30 0.0190(10) 0.0171(10) 0.0199(10) 0.0012(8) 0.0011(8) 0.0000(8) C31 0.0124(9) 0.0201(10) 0.0137(9) -0.0009(7) 0.0020(7) 0.0047(7) C32 0.0342(14) 0.0303(14) 0.0194(11) -0.0091(10) 0.0052(10) -0.0090(11) C33 0.0325(14) 0.0190(11) 0.0386(14) 0.0029(10) 0.0255(12) 0.0016(10) C34 0.164(7) 0.056(3) 0.203(8) -0.058(4) 0.170(7) -0.056(4) C35 0.0105(9) 0.0213(10) 0.0137(9) -0.0008(7) 0.0020(7) -0.0015(7) C36 0.0444(19) 0.063(2) 0.0167(12) -0.0070(13) 0.0108(12) 0.0066(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O13 2.3178(19) . ? Eu1 O10 2.3298(19) . ? Eu1 O11 2.350(2) . ? Eu1 O1 2.360(2) . ? Eu1 O7 2.3684(18) . ? Eu1 N1 2.595(2) . ? Eu1 N6 2.681(2) . ? Eu1 N2 2.735(2) . ? Eu1 Na2 3.8450(13) 1_545 ? Eu2 O14 2.3158(17) . ? Eu2 O5 2.3339(17) . ? Eu2 O12 2.338(2) . ? Eu2 O9 2.3695(19) . ? Eu2 O3 2.3850(17) . ? Eu2 N4 2.565(2) . ? Eu2 N3 2.681(2) . ? Eu2 N5 2.735(2) . ? Eu2 C31 3.170(2) . ? Eu2 C26 3.254(2) . ? Na2 O6 2.347(2) . ? Na2 O7 2.365(2) 1_565 ? Na2 O16 2.367(3) . ? Na2 O15 2.444(3) . ? Na2 Na1 3.3937(12) 1_565 ? Na1 O6 2.3654(18) 2_665 ? Na1 O15 2.401(2) 1_545 ? Na1 O8 2.4105(18) 2_655 ? Na1 Na2 3.3937(12) 2_665 ? O1 C24 1.268(3) . ? O1 Na2 2.520(2) 1_545 ? O2 C24 1.249(4) . ? O3 C26 1.269(3) . ? O4 C26 1.241(3) . ? O5 C28 1.275(3) . ? O6 C28 1.236(3) . ? O6 Na1 2.3654(18) 1_565 ? O7 C30 1.280(3) . ? O7 Na2 2.365(2) 1_545 ? O8 C30 1.239(3) . ? O9 C31 1.255(3) . ? O10 C31 1.253(3) . ? O11 C33 1.254(3) . ? O12 C33 1.213(3) . ? O13 C35 1.243(3) . ? O14 C35 1.249(3) . ? O15 Na1 2.401(2) 1_565 ? O15 H151 0.77(5) . ? O15 H152 0.66(5) . ? O16 H161 0.56(6) . ? O16 H162 0.95(5) . ? N1 C1 1.341(3) . ? N1 C5 1.345(3) . ? N2 C6 1.467(4) . ? N2 C23 1.483(3) . ? N2 C7 1.495(3) . ? N3 C25 1.475(3) . ? N3 C11 1.486(3) . ? N3 C10 1.489(3) . ? N4 C16 1.345(3) . ? N4 C12 1.347(3) . ? N5 C17 1.477(4) . ? N5 C27 1.491(3) . ? N5 C18 1.494(3) . ? N6 C29 1.474(3) . ? N6 C22 1.487(3) . ? N6 C21 1.491(3) . ? C1 C2 1.381(3) . ? C1 C22 1.500(3) . ? C2 C3 1.386(4) . ? C2 H2 0.9500 . ? C3 C4 1.376(4) . ? C3 H3 0.9500 . ? C4 C5 1.397(3) . ? C4 H4 0.9500 . ? C5 C6 1.506(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.469(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.194(3) . ? C9 C10 1.466(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.499(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.388(4) . ? C13 C14 1.383(4) . ? C13 H13 0.9500 . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 C16 1.386(4) . ? C15 H15 0.9500 . ? C16 C17 1.506(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.459(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.199(4) . ? C20 C21 1.465(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.511(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C25 C26 1.518(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 C28 1.513(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C29 C30 1.522(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 C32 1.498(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.495(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.507(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Eu1 O10 84.04(7) . . ? O13 Eu1 O11 106.27(10) . . ? O10 Eu1 O11 77.30(8) . . ? O13 Eu1 O1 139.95(7) . . ? O10 Eu1 O1 133.32(7) . . ? O11 Eu1 O1 75.41(8) . . ? O13 Eu1 O7 140.23(6) . . ? O10 Eu1 O7 80.71(8) . . ? O11 Eu1 O7 105.81(11) . . ? O1 Eu1 O7 71.40(7) . . ? O13 Eu1 N1 67.52(6) . . ? O10 Eu1 N1 137.86(7) . . ? O11 Eu1 N1 139.00(9) . . ? O1 Eu1 N1 85.04(7) . . ? O7 Eu1 N1 101.33(7) . . ? O13 Eu1 N6 77.68(6) . . ? O10 Eu1 N6 80.38(6) . . ? O11 Eu1 N6 156.71(8) . . ? O1 Eu1 N6 116.77(7) . . ? O7 Eu1 N6 63.69(6) . . ? N1 Eu1 N6 64.08(7) . . ? O13 Eu1 N2 74.93(6) . . ? O10 Eu1 N2 140.10(7) . . ? O11 Eu1 N2 76.68(9) . . ? O1 Eu1 N2 66.46(7) . . ? O7 Eu1 N2 135.64(7) . . ? N1 Eu1 N2 62.45(7) . . ? N6 Eu1 N2 125.83(6) . . ? O13 Eu1 Na2 173.14(5) . 1_545 ? O10 Eu1 Na2 99.06(6) . 1_545 ? O11 Eu1 Na2 80.44(9) . 1_545 ? O1 Eu1 Na2 39.51(5) . 1_545 ? O7 Eu1 Na2 35.64(5) . 1_545 ? N1 Eu1 Na2 106.56(5) . 1_545 ? N6 Eu1 Na2 96.73(5) . 1_545 ? N2 Eu1 Na2 105.79(5) . 1_545 ? O14 Eu2 O5 135.99(6) . . ? O14 Eu2 O12 91.02(8) . . ? O5 Eu2 O12 133.00(8) . . ? O14 Eu2 O9 110.16(7) . . ? O5 Eu2 O9 83.63(7) . . ? O12 Eu2 O9 78.50(7) . . ? O14 Eu2 O3 139.86(6) . . ? O5 Eu2 O3 68.28(6) . . ? O12 Eu2 O3 74.06(7) . . ? O9 Eu2 O3 103.15(7) . . ? O14 Eu2 N4 68.36(7) . . ? O5 Eu2 N4 74.85(7) . . ? O12 Eu2 N4 139.64(7) . . ? O9 Eu2 N4 140.39(7) . . ? O3 Eu2 N4 99.21(7) . . ? O14 Eu2 N3 77.46(6) . . ? O5 Eu2 N3 108.12(6) . . ? O12 Eu2 N3 77.12(7) . . ? O9 Eu2 N3 154.58(6) . . ? O3 Eu2 N3 63.07(6) . . ? N4 Eu2 N3 64.99(6) . . ? O14 Eu2 N5 76.26(6) . . ? O5 Eu2 N5 66.29(6) . . ? O12 Eu2 N5 146.17(7) . . ? O9 Eu2 N5 76.87(7) . . ? O3 Eu2 N5 134.28(6) . . ? N4 Eu2 N5 64.16(6) . . ? N3 Eu2 N5 128.35(6) . . ? O6 Na2 O7 90.80(8) . 1_565 ? O6 Na2 O16 164.08(10) . . ? O7 Na2 O16 91.03(11) 1_565 . ? O6 Na2 O15 81.52(8) . . ? O7 Na2 O15 102.86(8) 1_565 . ? O16 Na2 O15 82.66(9) . . ? O6 Na2 O1 113.50(8) . 1_565 ? O7 Na2 O1 68.70(7) 1_565 1_565 ? O16 Na2 O1 81.83(9) . 1_565 ? O15 Na2 O1 162.15(9) . 1_565 ? O6 Na1 O6 180.00(11) 2_665 1_545 ? O6 Na1 O15 82.04(7) 2_665 2_665 ? O6 Na1 O15 97.96(7) 1_545 2_665 ? O15 Na1 O15 180.00(14) 2_665 1_545 ? O6 Na1 O8 88.91(6) 2_665 . ? O6 Na1 O8 91.09(6) 1_545 . ? O15 Na1 O8 87.95(8) 2_665 . ? O15 Na1 O8 92.05(8) 1_545 . ? C24 O1 Eu1 125.89(18) . . ? C24 O1 Na2 128.5(2) . 1_545 ? Eu1 O1 Na2 103.93(8) . 1_545 ? C26 O3 Eu2 122.91(15) . . ? C28 O5 Eu2 128.24(17) . . ? C28 O6 Na2 132.18(17) . . ? C28 O6 Na1 128.86(16) . 1_565 ? Na2 O6 Na1 92.14(7) . 1_565 ? C30 O7 Na2 125.29(16) . 1_545 ? C30 O7 Eu1 126.01(16) . . ? Na2 O7 Eu1 108.66(8) 1_545 . ? C30 O8 Na1 132.34(17) . . ? C31 O9 Eu2 118.78(16) . . ? C31 O10 Eu1 154.51(18) . . ? C33 O11 Eu1 134.4(2) . . ? C33 O12 Eu2 164.8(2) . . ? C35 O13 Eu1 146.77(16) . . ? C35 O14 Eu2 154.27(16) . . ? Na1 O15 Na2 88.93(8) 1_565 . ? Na1 O15 H151 142(3) 1_565 . ? Na2 O15 H151 110(3) . . ? Na1 O15 H152 99(4) 1_565 . ? Na2 O15 H152 98(4) . . ? H151 O15 H152 110(5) . . ? Na2 O16 H161 134(7) . . ? Na2 O16 H162 117(3) . . ? H161 O16 H162 91(7) . . ? C1 N1 C5 118.5(2) . . ? C1 N1 Eu1 118.80(16) . . ? C5 N1 Eu1 121.11(16) . . ? C6 N2 C23 108.9(2) . . ? C6 N2 C7 109.0(2) . . ? C23 N2 C7 107.1(2) . . ? C6 N2 Eu1 109.93(15) . . ? C23 N2 Eu1 107.30(15) . . ? C7 N2 Eu1 114.43(15) . . ? C25 N3 C11 108.26(18) . . ? C25 N3 C10 109.71(18) . . ? C11 N3 C10 108.44(19) . . ? C25 N3 Eu2 107.11(14) . . ? C11 N3 Eu2 104.33(13) . . ? C10 N3 Eu2 118.52(13) . . ? C16 N4 C12 119.3(2) . . ? C16 N4 Eu2 121.79(16) . . ? C12 N4 Eu2 118.68(16) . . ? C17 N5 C27 110.2(2) . . ? C17 N5 C18 108.6(2) . . ? C27 N5 C18 105.93(19) . . ? C17 N5 Eu2 108.59(14) . . ? C27 N5 Eu2 107.84(15) . . ? C18 N5 Eu2 115.59(14) . . ? C29 N6 C22 108.17(19) . . ? C29 N6 C21 109.89(19) . . ? C22 N6 C21 108.68(19) . . ? C29 N6 Eu1 107.19(14) . . ? C22 N6 Eu1 104.15(14) . . ? C21 N6 Eu1 118.27(14) . . ? N1 C1 C2 123.0(2) . . ? N1 C1 C22 115.2(2) . . ? C2 C1 C22 121.8(2) . . ? C1 C2 C3 118.5(2) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 119.1(2) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 119.3(2) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 121.5(2) . . ? N1 C5 C6 118.1(2) . . ? C4 C5 C6 120.3(2) . . ? N2 C6 C5 112.5(2) . . ? N2 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N2 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C8 C7 N2 114.9(2) . . ? C8 C7 H7A 108.6 . . ? N2 C7 H7A 108.6 . . ? C8 C7 H7B 108.6 . . ? N2 C7 H7B 108.6 . . ? H7A C7 H7B 107.5 . . ? C9 C8 C7 174.2(2) . . ? C8 C9 C10 178.1(2) . . ? C9 C10 N3 113.12(19) . . ? C9 C10 H10A 109.0 . . ? N3 C10 H10A 109.0 . . ? C9 C10 H10B 109.0 . . ? N3 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? N3 C11 C12 112.26(18) . . ? N3 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N3 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N4 C12 C13 122.1(2) . . ? N4 C12 C11 116.4(2) . . ? C13 C12 C11 121.5(2) . . ? C14 C13 C12 118.4(2) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 119.7(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 119.0(3) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? N4 C16 C15 121.5(2) . . ? N4 C16 C17 117.6(2) . . ? C15 C16 C17 120.7(2) . . ? N5 C17 C16 113.6(2) . . ? N5 C17 H17A 108.8 . . ? C16 C17 H17A 108.8 . . ? N5 C17 H17B 108.8 . . ? C16 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C19 C18 N5 116.2(2) . . ? C19 C18 H18A 108.2 . . ? N5 C18 H18A 108.2 . . ? C19 C18 H18B 108.2 . . ? N5 C18 H18B 108.2 . . ? H18A C18 H18B 107.4 . . ? C20 C19 C18 171.5(2) . . ? C19 C20 C21 176.7(2) . . ? C20 C21 N6 112.45(19) . . ? C20 C21 H21A 109.1 . . ? N6 C21 H21A 109.1 . . ? C20 C21 H21B 109.1 . . ? N6 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? N6 C22 C1 110.45(19) . . ? N6 C22 H22A 109.6 . . ? C1 C22 H22A 109.6 . . ? N6 C22 H22B 109.6 . . ? C1 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? N2 C23 C24 113.7(2) . . ? N2 C23 H23A 108.8 . . ? C24 C23 H23A 108.8 . . ? N2 C23 H23B 108.8 . . ? C24 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? O2 C24 O1 124.9(3) . . ? O2 C24 C23 117.5(3) . . ? O1 C24 C23 117.5(3) . . ? N3 C25 C26 111.69(19) . . ? N3 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? N3 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? O4 C26 O3 125.0(2) . . ? O4 C26 C25 117.9(2) . . ? O3 C26 C25 117.1(2) . . ? N5 C27 C28 114.9(2) . . ? N5 C27 H27A 108.5 . . ? C28 C27 H27A 108.5 . . ? N5 C27 H27B 108.5 . . ? C28 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? O6 C28 O5 124.9(2) . . ? O6 C28 C27 118.3(2) . . ? O5 C28 C27 116.6(2) . . ? N6 C29 C30 111.4(2) . . ? N6 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? N6 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? O8 C30 O7 125.5(2) . . ? O8 C30 C29 118.0(2) . . ? O7 C30 C29 116.5(2) . . ? O10 C31 O9 122.5(2) . . ? O10 C31 C32 118.8(2) . . ? O9 C31 C32 118.8(2) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O12 C33 O11 124.8(3) . . ? O12 C33 C34 119.9(3) . . ? O11 C33 C34 115.3(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O13 C35 O14 125.0(2) . . ? O13 C35 C36 117.2(2) . . ? O14 C35 C36 117.8(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 32.01 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.396 _refine_diff_density_min -2.893 _refine_diff_density_rms 0.134 #===END